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Water → 1-[4-(3-Mercapto-2-mercaptomethyl-2-methyl-propylthio)-phenyl]-2-methyl-2-morpholin-4-yl-propan-1-one

HRID 376972
ノート
印刷プレビュー

反応式

HRID 376972 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:18])[C:9]([CH3:17])([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH3:10])=[CH:4][CH:3]=1.[SH:19][CH2:20][C:21]([CH2:25][SH:26])([CH2:23][SH:24])[CH3:22].[H-].[Na+].O>CN(C)C=O>[SH:19][CH2:20][C:21]([CH2:25][SH:26])([CH3:22])[CH2:23][S:24][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:18])[C:9]([CH3:17])([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[CH3:10])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 115138141,3-Propanedithiol, 2-(mercaptomethyl)-2-methyl-HCID 154053051-(4-Fluorphenyl)-2-methyl-2-morpholino-1-propanone

生成物 1

HCID 193606041-[4-(3-Mercapto-2-mercaptomethyl-2-methyl-propylthio)-phenyl]-2-methyl-2-morpholin-4-yl-propan-1-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

3.6 g (14.3 mmol) of 1-(4-fluorophenyl)-2-methyl-2-morpholin-4-yl-propan-1-one and 12 g (71.3 mmol) of 1,1,1-trismercaptomethylethane are dissolved in 70 ml of dry dimethylformamide, and 28.6 mmol of sodium hydride are added. The solution is stirred at room temperature for 2 h. Then the solution is poured into water. The crude product is extracted with methylene chloride, washed with water, dried over MgSO4, and concentrated. The residue is purified by column chromatography on silica gel with methylene chloride as an eluent. The structure is confirmed by the 1H-NMR spectrum (CDCl3): δ [ppm] 1.12 (s, 3H), 1.30 (t, 2H), 1.31 (s, 6H), 2.57 (t, 4H), 2.62-2.72 (m, 4H), 3.14 (s, 2H), 3.69 (t, 4H), 7.33 (d, 2H), 8.49 (d, 2H).

後処理

  1. extractionThe crude product is extracted with methylene chloride
  2. washwashed with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe residue is purified by column chromatography on silica gel with methylene chloride as an eluent

出典と根拠

ORDレコード
ord-1aebfafd823e4b548631e7f95a3d8730
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06022906

反応ノート

読み込み中…

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