Phosgene → 2H-Indazole, 3-chloro-2-(4-chloro-2-fluorophenyl)-4,5,6,7-tetrahydro-

HRID 2083123노트

반응식

HRID 2083123 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>ClC1C=CC=CC=1>[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]=1

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 227482812-(4-Chloro-2-fluorophenyl)-1,2,4,5,6,7-hexahydro-3H-indazol-3-one

생성물 1

HCID 946072H-Indazole, 3-chloro-2-(4-chloro-2-fluorophenyl)-4,5,6,7-tetrahydro-

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

반응 조건

온도
25 °C

실험 절차

Ten parts of 2-(4-chloro-2-fluorophenyl)-1,2,4,5,6,7-hexahydro-3H-indazol-3-one and 50 parts of chlorobenzene were charged to a Hastalloy C-lined shaker tube. The vessel was closed, charged with 10 parts of phosgene from a pressurized cylinder, and heated to 130° with constant shaking for 4 hours. The vessel was cooled to 25° C, vented, opened and discharged. The product mixture was evaporated under reduced pressure to give 10.1 parts of 2-(4-chloro-2-fluorophenyl)-3-chloro,4,5,6,7-tetrahydro-2H-indazole, m.p. 82°-85°. (90.7% pure as determined by gas chromatography).

후처리

  1. customThe vessel was closed
  2. temperatureheated to 130°
  3. customThe product mixture was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-359ed1f213c6479b810bbaa326bd2452
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04084055

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