Diketene → HCID 20534014, 화합물

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[NH2:1][C:2]1[C:3](=[O:10])[CH:4]=[CH:5][C:6]([Cl:9])=[CH:7][CH:8]=1.[CH2:11]=[C:12]1[O:16][C:14](=[O:15])[CH2:13]1>>[Cl:9][C:6]1[CH:5]=[CH:4][C:3](=[O:10])[C:2]([NH:1][C:14](=[O:15])[CH2:13][C:12](=[O:16])[CH3:11])=[CH:8][CH:7]=1

참가 물질

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HCID 12661Diketene

HCID 12557673HCID 12557673, 화합물

생성물 1

HCID 20534014HCID 20534014, 화합물

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온도: 100 °C

실험 절차

A mixture of 2-amino-5-chloro-2,4,6-cycloheptatrien-1-one (1.55 g, described in example 9) and diketene (5 ml) were heated at 100° C. for 1 hr. The mixture was cooled and then purified by chromatography on silica gel using chloroform as the eluant. The appropriate fractions were pooled and the residue was crystallized from diethyl ether to give 650 mg of 1-[(4-chloro-7-oxo-1,3,5-cycloheptatrien-1-yl)amino]-1,3-butanedione, nmr (DMSO-d6) δ2.17 (s, 3H), 3.85 (s, 2H), 7.3 (m, 3H), 8.7 (d, 1H), 10.75 (s, 1H).

후처리

temperatureThe mixture was cooled
custompurified by chromatography on silica gel
customthe residue was crystallized from diethyl ether

출처 및 근거

ORD 기록: ord-26a39316d38249cb925e9e007aff87e0
출처 데이터셋: uspto-grants-1982_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04337265

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