Water → 5-(1-Methylethyl)-3-[(1-methylpiperidin-4-yl)sulfonyl]-1H-indole

HRID 36889노트

반응식

HRID 36889 반응식
S([O-])(O[O-])(=O)=[O:2].[K+].[K+].[CH3:9][CH:10]([C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[NH:17][CH:16]=[C:15]2[S:21][CH:22]1[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]1)[CH3:11].[OH2:29]>>[CH3:11][CH:10]([C:12]1[CH:13]=[C:14]2[C:18](=[CH:19][CH:20]=1)[NH:17][CH:16]=[C:15]2[S:21]([CH:22]1[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]1)(=[O:2])=[O:29])[CH3:9]

참가 물질

4

반응물 3

HCID 962WaterHCID 10313463Potassium peroxymonosulphateHCID 199366285-(1-methylethyl)-3-[(1-methylpiperidin-4-yl)thio]-1H-indole

생성물 1

HCID 199366475-(1-Methylethyl)-3-[(1-methylpiperidin-4-yl)sulfonyl]-1H-indole

실험 절차

A solution of potassium peroxymonosulfate (49.5% KHSO5, 21.2 g) in water (95 ml) is added drop-wise at 0° C. to a methanolic solution (95 ml) of 5-(1-methylethyl)-3-[(1-methylpiperidin-4-yl)thio]-1H-indole (7.5 g, prepared in Example 43). After 4 hours at room temperature, the white precipitate is filtered off and the filtrate is concentrated, rendered basic with sodium carbonate and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and concentrated. 5-(1-Methylethyl)-3-[(1-methylpiperidin-4-yl)sulfonyl]-1H-indole (2.4 g) is obtained after purification on silica gel (eluent: CH2Cl2 /iPrNH2 95/5).

후처리

  1. filtrationthe white precipitate is filtered off
  2. concentrationthe filtrate is concentrated
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ffc00cac7a57496b9c1e95ac2274109a
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418242

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