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

HRID 36889ノート

反応式

HRID 36889 の反応式
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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ffc00cac7a57496b9c1e95ac2274109a
出典データセット
uspto-grants-1995_05
特許番号
US05418242

反応ノート

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