The Solubility of Hydrogen in Liquid Sodium<sup>1</sup>

McClure, D.; Halsey, G. D.

doi:10.1021/j100894a049

Cited by 21 publications

(2 citation statements)

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“…Column chromatography was performed on silica gel (various grades). Triplet extinction coefficients over the laser action spectral region of the dye were measured at the temperature of liquid nitrogen by equipment previously described [28] using McClure's method [29]. Molecular mechanics calculations were performed on a MicroVAX 2000 computer with Evans and Sutherland PS390 graphics display using the BIOGRAF [30] software package.…”

Section: Methodsmentioning

confidence: 99%

“…Dehydrogenation of syn4 tetrameth-y1ene)bimane 26 by treatment with dichlorodicyanobenzoquinone (DDQ) gave syn-(benzo.tetrameth-y1ene)biniane 27 (58%) and syn-(benzo)l?imane 28 (29%). Bromination of the bimane 26 gave a dibromide 29 (92%) that was also converted bt treatment with DDQ to syn-(benzo)bimane 28. Trealment with palladium (1 0%) on charcoal dehydrogenated 5,6,10, I I -tetrahydro-7H,9H-benz [6,7] indazol [ I , 2-a]benz[g]indazol-7,9-dione 35 to syn-(a-naphtho)bimane 36 (71%).…”

Section: -Carboethox~methvl-4-chloro-2-pyrazolin-5-one 1 Oc Syn-(mementioning

confidence: 99%

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Bimanes (1,5‐diazabicyclo[3.3.0]octadienediones): Laser activity in syn‐bimanes

Stevens

Boyer

Lau

et al. 1990

Heteroatom Chemistry

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The conversion of 3‐methyl‐4‐benzyl‐4‐chloro‐2‐pyrazolin‐5‐one 10b was catalyzed by a mixture of potassium fluoride and alumina to give syn‐(methyl, benzyl)bimane 6 (62%) without detectable formation of the anti isomer,A6 [a 1 : 1 mixture (87%) of the isomers 6 and A6 was obtained when the catalyst was potassium carbonate]. In a similar reaction syn‐(methyl,carboethoxymethyl)bimane 7 (15%) with the anti isomer A7 (36%) was obtained from 3‐methyl‐4‐carboethoxymethyl‐4‐chloro‐2‐pyrazolin‐5‐one 10c. syn‐(Methyl, β‐acetoxyethyl)bimane 8 (70%) was obtained from 3‐methyl‐4‐β‐acetoxyethyl‐4‐chloro‐2‐pyrazolin‐5‐one 10d (potassium carbonate catalysis) and was converted by hydrolysis to syn‐(methyl, β‐hydroxyethyl)bimane 9 (40%). Acetyl nitrate (nitric acid in acetic anhydride) converted anti‐(amino,hydrogen)bimane 11 to anti‐(amino,nitro)bimane 15 (91%), anti‐(methyl,hydrogen)bimane 13 to anti‐(methyl,nitro)(methyl,hydrogen)bimane 16 (57%), and degraded syn‐(methyl,hydrogen)bimane 12 to an intractable mixture. Treatment with trimethyl phosphite converted syn‐(bromomethyl,methyl)bimane 17 to syn‐(dimethoxyphosphinylmethyl,methyl)bimane 18 (78%) that was further converted to syn‐(styryl,methyl)bimane 19 (29%) in a condensation reaction with benzaldehyde. Treatment with acryloyl chloride converted syn‐(hydroxymethyl,methyl)bimane 20 to its acrylate ester 21 (22%). Stoichiometric bromination of syn‐(methyl,methyl)bimane 1 gave a monobromo derivative that was converted in situ by treatment with potassium acetate to syn‐(acetoxymethyl,methyl)(methyl,methyl)bimane 47. N‐Amino‐μ‐amino‐syn‐(methylene,methyl)bimane 24 (68%) was obtained from a reaction between the dibromide 17 and hydrazine. Derivatives of the hydrazine 24 included a perchlorate salt and a hydrazone 25 derived from acetone. Dehydrogenation of syn‐(tetramethylene)bimane 26 by treatment with dichlorodicyanobenzoquinone (DDQ) gave syn‐(benzo,tetramethylene)bimane 27 (58%) and syn‐(benzo)bimane 28 (29%). Bromination of the bimane 26 gave a dibromide 29 (92%) that was also converted by treatment with DDQ to syn‐(benzo)bimane 28. Treatment with palladium (10%) on charcoal dehydrogenated 5, 6, 10, 11‐tetrahydro‐7H,9H‐benz [6, 7] indazol [1, 2a]benz[g]indazol‐7,9‐dione 35 to syn‐(α‐naphtho)bimane 36 (71%). The bimane 35 was prepared from 1,2,3,4‐tetrahydro‐1‐oxo‐2‐naphthoate 37 by stepwise treatment with hydrazine to give 1,2,4,5‐tetrahydro‐3H‐benz[g]indazol‐3‐one 38, followed by chlorine to give 3a‐chloro‐2,3a,4,5‐tetrahydro‐3H‐benz[g]indazol‐3‐one 39, and base. Dehydrogenation over palladium converted the indazolone 34 to 1H‐benz[g] indazol‐3‐ol 36. Helicity for the hexacyclic syn‐(α‐naphtho)bimane 36 was confirmed by an analysis based on molecular modeling. The relative efficiencies (RE) for laser activity in the spectral region 500–530 nm were obtained for 37 syn‐bimanes by reference to coumarin 30 (RE 100): RE > 80 for syn‐bimanes 3, 5, 18, and μ‐(dicarbomethoxy)methylene‐syn‐(methylene,methyl)bimane 22: RE 20–80: for syn‐bimanes 1,2,4,20,24,26, and μ‐thia‐s...

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Section: Methodsmentioning

confidence: 99%

Section: -Carboethox~methvl-4-chloro-2-pyrazolin-5-one 1 Oc Syn-(mementioning

confidence: 99%

Bimanes (1,5‐diazabicyclo[3.3.0]octadienediones): Laser activity in syn‐bimanes

Stevens

Boyer

Lau

et al. 1990

Heteroatom Chemistry

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Liquid Mixtures of Sodium and Sodium Hydride at High Pressures and Temperatures

Klostermeier

Franck

1982

Ber Bunsenges Phys Chem

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The hydrogen pressure in equilibrium with liquid phases of the system sodium‐sodium hydride has been measured from 650 to 900 °C and up to 900 bar. A detailed description of the apparatus is given. The autoclave was of a nickel base superalloy and contained an outer and an inner compartment with equilibrated hydrogen pressures. At 900°C and 650 bar the maximum solubility of NaH in liquid Na is 19 mole percent. Sieverts' law is closely obeyed to 5% NaH. Sodium solubility in the liquid NaH is below 2%. The melting point of NaH was found at 632 °C and 106 bar, the enthalpy and entropy of fusion as 26.2 ± 0.7 kJ mol−1 and 29.0 ± 0.8 JK−1 mol−1. The enthalpy of solution of liquid NaH in liquid Na is 27.4 kJ mol−1. Equations and data for solubility, activity coefficients etc. of NaH are given. The critical solution point for Na and NaH is estimated to be at 1500 ± 70 K, 2500 ± 600 bar and x(NaH) = 0.65 ± 0.05.

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