HCID 57973773、化合物 → HCID 11589768、化合物

HRID 1863954ノート

反応式

HRID 1863954 の反応式
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

参加物

4

反応物 2

HCID 57973773HCID 57973773、化合物2 回HCID 57973796HCID 57973796、化合物2 回

生成物 1

HCID 11589768HCID 11589768、化合物

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

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.

後処理

  1. temperatureat reflux for 18 h

出典と根拠

ORDレコード
ord-0478d6bd60f84a1caf4314db5c0fd9e2
出典データセット
uspto-grants-2009_12
特許番号
US07625888B2

反応ノート

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