Potassium hydroxy sulfite → HCID 58456640, compound

HRID 41870Notes

Reaction equation

HRID 41870 reaction equation
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[C:9]([S:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[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:33]3[CH2:38][CH2:37][CH2:36][C@H:34]3[N:35]=[C:3]12.[OH:39]OS([O-])=O.[K+]>CC#N.CO>[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[C:9]([S:26]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[O:39])[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:33]3[CH2:38][CH2:37][CH2:36][C@H:34]3[N:35]=[C:3]12

Participants

5

Reactant 2

HCID 23707502Potassium hydroxy sulfiteHCID 58456655HCID 58456655, compound

Product 1

HCID 58456640HCID 58456640, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 6342AcetonitrileSolvent

Procedure

(6aR,9aS)-5,6a,7,8,9,9a-hexahydro-5-methyl-3-(phenylthio)-2-(4-(6-fluoropyridin-2-yl)benzyl)-cyclopent[4,5]imidazo[1,2-a]pyrazolo[4,3-e]pyrimidin-4(2H)-one (12 mg, 0.023 mmol) is dissolved in CH3CN (2 mL) and CH3OH (2 mL), and then an aqueous solution of oxone is added. The reaction mixture is stirred at room temperature for a week, and then purified by a semi-preparative HPLC to give pure product as white solids. MS (ESI) m/z 541.2 [M+H]+.

Workup

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

Sources & evidence

ORD record
ord-2022d11d044944478ba17960fbd01d7c
Source dataset
uspto-grants-2013_09
Patent number
US08536159B2

Reaction notes

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