Abstract:56 Bericht: Allgem. analyt. Methoden etc. 2. Auf angewand~e Chemie beziigl. ~ber eia Irrometer wird yon O. M a y e r 1) berichtet. Dieses zur Bestimmung des spezifischeu Gewichts des Harnes dienende, etwa 16 c~ lange Ar~tometer wird yon Johannes Greiner, Mt~nchen, aus ~orma!glas angefertigt und tr~igt eine yon 1,000--1,045 reiehende, 6,2 c~ lange Skala; auf dieser kOnn6n noch 0,0005 Grade abgelesen werden, da der zwischen den einzelnen Teilstriehen liegende Raum 1,4 rnm betr~tgt. Die Eichung der Skala bezieht … Show more
Section: -Zsopropyliden-2-cyclopen1en-l-on (5; Im Gemisch Mit 8)unclassified
“…I-(2-Meihylphenyl)-3-irimethyl.silyl-Z-propin-I-on (41). Behandlung von 20,O g (129 mmol) o-Methylbenzoyl-chlorid [40] mit 22,l g (130 mmol) Bis(trimethylsily1)acetylen analog zu [2], jedoch bei -60", lieferte nach KR.-Destillation des Rohproduktes bei 100"/0,06Torr 24.5 g (88 %) 41 als hellgelbes 0 1 . UV (EtOH): 267 (13900), 244 (sh, 8200), 222 (7600).…”
Section: -Zsopropyliden-2-cyclopen1en-l-on (5; Im Gemisch Mit 8)unclassified
The Gas-Flow Thermolysis of 1-Isobutenyl Alkynyl and 2-Methylphenyl Alkynyl Ketones. Synthesis of Methylenomycin BThe gas-flow thermolysis of I-isobutenyl alkynyl or 2-methylphenyl alkynyl ketones were found to lead to phenols and cyclopentenones or to naphthols and indanones, respectively. These conversions involve two cyclization processes so far unknown with a-alkynones; they are interpreted as intramolecular additions of an allylic or a benzylic C,H bond to a triple bond which may occur in two directions. In addition, the cyclopentenones formed by the a-alkynone cyclization, a known carbene process yielding 5-rings, were also found. The available evidence ruled out a carbene process yielding 6-rings. The addition process yielding 5-rings was applied to a short (but low yield) synthesis of methylenomycin B.
Section: -Zsopropyliden-2-cyclopen1en-l-on (5; Im Gemisch Mit 8)unclassified
“…I-(2-Meihylphenyl)-3-irimethyl.silyl-Z-propin-I-on (41). Behandlung von 20,O g (129 mmol) o-Methylbenzoyl-chlorid [40] mit 22,l g (130 mmol) Bis(trimethylsily1)acetylen analog zu [2], jedoch bei -60", lieferte nach KR.-Destillation des Rohproduktes bei 100"/0,06Torr 24.5 g (88 %) 41 als hellgelbes 0 1 . UV (EtOH): 267 (13900), 244 (sh, 8200), 222 (7600).…”
Section: -Zsopropyliden-2-cyclopen1en-l-on (5; Im Gemisch Mit 8)unclassified
The Gas-Flow Thermolysis of 1-Isobutenyl Alkynyl and 2-Methylphenyl Alkynyl Ketones. Synthesis of Methylenomycin BThe gas-flow thermolysis of I-isobutenyl alkynyl or 2-methylphenyl alkynyl ketones were found to lead to phenols and cyclopentenones or to naphthols and indanones, respectively. These conversions involve two cyclization processes so far unknown with a-alkynones; they are interpreted as intramolecular additions of an allylic or a benzylic C,H bond to a triple bond which may occur in two directions. In addition, the cyclopentenones formed by the a-alkynone cyclization, a known carbene process yielding 5-rings, were also found. The available evidence ruled out a carbene process yielding 6-rings. The addition process yielding 5-rings was applied to a short (but low yield) synthesis of methylenomycin B.
“…The oxidation took place more readily than did the oxidation of 4-chloro-l,3-dimethylbenzene, although the yields were nearly the same. No description of 2-chloroisophthalic acid could be found in the literature, although 2-bromoisophthalic acid (12) and 2-iodoisophthalic acid (13) have been reported. The condensation with p-toluidine to form 2-(p-rnethylphenylamino)-isophthalic acid (XXII) required less rigorous conditions than the condensation involving 4-chloroisophthalic acid.…”
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