Acetonitrile → HCID 46239062、化合物

HRID 41874ノート

反応式

HRID 41874 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[C:9](SC)[N:10]([CH2:12][C:13]3[CH:18]=[CH:17][C:16]([C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[N:20]=4)=[CH:15][CH:14]=3)[N:11]=[C:5]2[N:4]2[C@H:28]3[CH2:33][CH2:32][CH2:31][C@H:29]3[N:30]=[C:3]12.O[O:35][S:36]([O-:38])=O.[K+].[CH3:40]C#N>CO>[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[C:9]([S:36]([CH3:40])(=[O:38])=[O:35])[N:10]([CH2:12][C:13]3[CH:14]=[CH:15][C:16]([C:19]4[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[N:20]=4)=[CH:17][CH:18]=3)[N:11]=[C:5]2[N:4]2[C@H:28]3[CH2:33][CH2:32][CH2:31][C@H:29]3[N:30]=[C:3]12

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 23707502Potassium hydroxy sulfiteHCID 58456641HCID 58456641、化合物

生成物 1

HCID 46239062HCID 46239062、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(6aR,9aS)-5,6a,7,8,9,9a-hexahydro-5-methyl-3-(methylthio)-2-(4-(6-fluoropyridin-2-yl)benzyl)-cyclopent[4,5]imidazo[1,2-a]pyrazolo[4,3-e]pyrimidin-4(2H)-one (35.2 mg, 0.076 mmol) is dissolved in CH3CN (0.5 mL) and CH3OH (2 mL), and then an aqueous solution of oxone (139 mg, 0.226 mmol) is added. The reaction mixture is stirred at room temperature for 2 days, and then purified by a semi-preparative HPLC to give pure product as white solids. MS (ESI) m/z 495.2 [M+H]+.

後処理

  1. custompurified by a semi-preparative HPLC
  2. customto give pure product as white solids

出典と根拠

ORDレコード
ord-f73c338e0b9c4619908dfe5c8a124e2e
出典データセット
uspto-grants-2013_09
特許番号
US08536159B2

反応ノート

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