HCID 57973773, 화합물 → HCID 11589768, 화합물

HRID 1863954노트

반응식

HRID 1863954 반응식
C(OC(=O)[NH:7][C@H:8]([CH2:14][C:15]1[CH:20]=[C:19]([F:21])[C:18]([F:22])=[CH:17][C:16]=1[F:23])[CH2:9][C:10]([NH:12][NH2:13])=O)(C)(C)C.[F:25][C:26]([F:38])([F:37])[C:27]1[N:36]=[C:30]2[C:31](=S)[NH:32][CH2:33][CH2:34][N:29]2[N:28]=1>COCCO>[F:23][C:16]1[CH:17]=[C:18]([F:22])[C:19]([F:21])=[CH:20][C:15]=1[CH2:14][C@@H:8]([NH2:7])[CH2:9][C:10]1[N:32]2[C:31]([C:30]3[N:29]([N:28]=[C:27]([C:26]([F:38])([F:37])[F:25])[N:36]=3)[CH2:34][CH2:33]2)=[N:13][N:12]=1

참가 물질

4

반응물 2

HCID 57973773HCID 57973773, 화합물2회HCID 57973796HCID 57973796, 화합물2회

생성물 1

HCID 11589768HCID 11589768, 화합물

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

실험 절차

A mixture of 208 mg (0.6 mmol) of of tert-butyl[(1R)-3-hydrazino-3-oxo-1-(2,4,5-trifluorobenzyl)propyl]carbamate (Intermediate 4), 100 mg (0.45 mmol) of 2-(trifluoromethyl)-6,7-dihydro[1,2,4]triazolo[1,5-a]pyrazine-8(5H)-thione (Intermediate 7), and 5 mL of 2-methoxyethanol was stirred at reflux for 18 h, resulting primarily in ring closure of the initial adduct as well as loss of the Boc group. The cooled solution was purified by preparative HPLC (C18 reverse phase column, 30-75% acetonitrile in water containing 0.05% trifluoroacetic acid) to afford the title compound.

후처리

  1. temperatureat reflux for 18 h

출처 및 근거

ORD 기록
ord-0478d6bd60f84a1caf4314db5c0fd9e2
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625888B2

반응 노트

불러오는 중…