On the origin of the large refractive index change in photolyzed PbI_2 films*

Synthesis of 3‐substituted‐4‐methyl‐5‐acetyl‐4‐thiazoline‐2‐thione

“…Varian-MAT CH-7A mass spectrometer operating at an ionizing potential of 70 eV using a direct insertion probe technique with a source temperature at 250'. To a stirred slurry at 0" containing 0.25 mole of potassium dimethylaminodithiocarbamate [8] potassium 4-morpholinodithiocarbamate 181 potassium I-piperidinodithiocarbamate [8] or potassium hexahydro-l-(1Htazepinedithiocarbamate [8] in 400 ml of ethanol, 33.7 g (0.25 mole) of 3-chloro-2,4-pentanedione [5] was added in one portion. An exothermic reaction occurred causing a temperature rise from 0" to 25" over a 1 minute period.…”

“…The data are summarized in Table 1. ( To a stirred slurry at 20" comprising 0.25 mole of the same potassium salts listed above in 300 ml of ethanol, 33.7 g (0.25 mole) of 3-chloro-2.4pentanedione [5] was added in one portion. An exothermic reaction occurred causing a temperature rise from 20" to 50'.…”

“…The reaction of potassium salts [RNHC(=S)SK], R = -N(CH,),, morpholino, piperidino, or hexahydro-1-( 1H)azepinyl] in ethanol with 3-chloro-2,4-pentanedione [5] at 25-30' afforded 1-acetylacetonyl]dimethylaminodithiocarbamate (l), 1-acetylacetonyl4-morpholinodithiocarbamate (2), 1-acetylacetonyl 1-piperidinodithiocarbamate (3), 1-acetylacetonyl hexahydro-l(1H)azepinedithiocarbamate (4), respectively (Table 1). However, under refluxing temperatures (78-80°), the same reactants gave the heterocyclic compounds, 3-dimethylamino-4-methyl-5-acetyl-4-thiazoline-2-thione (5), 3-morpholino-4-methyI-5-acetyl-4-thiazoline-2-thione (6), 3-piperidino-4-methyl-5-acetyl-4-thiazoline-2-thione (7) and 3-(hexahydro-l-(lH)azepinyl)-4-methyl-5-acetyl-4-thiazoline-2-thione (8), respectively ( Table 2).…”