Phosgene → 2H-Indazole, 3-chloro-2-(4-chloro-2-fluorophenyl)-4,5,6,7-tetrahydro-
반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16](=O)[C:15]3[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=3[NH:9]2)=[C:4]([F:18])[CH:3]=1.C(Cl)([Cl:21])=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16]([Cl:21])=[C:15]3[C:10]([CH2:11][CH2:12][CH2:13][CH2:14]3)=[N:9]2)=[C:4]([F:18])[CH:3]=1참가 물질
실험 절차
One hundred parts of 2-(4-chloro-2-fluorophenyl)-1,2,4,5,6,7-hexahydro-3H-indazol-3-one was heated under a nitrogen atmosphere (nitrogen was slowly passed through the system at atmospheric pressure) in a 3-neck, round-bottomed flask, fitted with a mechanical stirrer, dry ice condenser, an addition funnel with a gas-inlet and dry ice condenser above it. Phosgene was condensed into the addition funnel from a pressurized cylinder, and 44 parts of phosgene was added dropwise over 2 hours, maintaining a temperature of 178°-180° in the reaction mixture for the first 11/2 hours and allowing it to fall to 135° during the last 1/2 hour. The dry ice in the condenser was removed and the excess phosgene was passed through a 10% sodium hydroxide solution as it evaporated. The reaction mixture was poured out into a pan and allowed to cool. There was obtained 100.6 parts of 2-(4-chloro-2-fluorophenyl)-3-chloro-4,5,6,7-tetrahydro-2H-indazole, m.p. 81°-85° (80.4% pure as determined by gas chromatography).
후처리
- customfitted with a mechanical stirrer, dry ice condenser, an addition funnel with a gas-inlet and dry ice condenser above it
- additionwas added dropwise over 2 hours
- temperaturemaintaining a temperature of 178°-180° in the reaction mixture for the first 11/2 hours
- customto fall to 135° during the last 1/2 hour
- customThe dry ice in the condenser was removed
- customevaporated
- additionThe reaction mixture was poured out into a pan
- temperatureto cool
출처 및 근거
- ORD 기록
- ord-6f25b9cfe63343c8b71bc7bbf7763a7d
- 출처 데이터셋
- uspto-grants-1978_04
- 특허 번호
- US04084055
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