Acetonitrile → HCID 46239062, 화합물

HRID 41874노트

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HRID 41874 반응식
[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

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 23707502Potassium hydroxy sulfiteHCID 58456641HCID 58456641, 화합물

생성물 1

HCID 46239062HCID 46239062, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(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]+.

후처리

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

출처 및 근거

ORD 기록
ord-f73c338e0b9c4619908dfe5c8a124e2e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536159B2

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