Dicyclohexylcarbodiimide → HCID 54392109、化合物

HRID 2226578ノート

反応式

HRID 2226578 の反応式
C1(N=C=NC2CCCCC2)CCCCC1.[CH2:16]([O:19][C:20](=[O:27])[C@@H:21]([OH:26])[CH2:22][S:23][CH2:24][CH3:25])[CH:17]=[CH2:18].[C:28]([S:31][CH2:32][C@@H:33]([CH3:37])[C:34](O)=[O:35])(=[O:30])[CH3:29]>ClCCl.CN(C)C1C=CN=CC=1>[CH2:16]([O:19][C:20](=[O:27])[C@@H:21]([O:26][C:34](=[O:35])[C@H:33]([CH3:37])[CH2:32][S:31][C:28](=[O:30])[CH3:29])[CH2:22][S:23][CH2:24][CH3:25])[CH:17]=[CH2:18]

参加物

6

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 2724506D-beta-acetylthioisobutyric acidHCID 54445895HCID 54445895、化合物

生成物 1

HCID 54392109HCID 54392109、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

Dicyclohexylcarbodiimide (1.13 g, 5.5 mmol) in dichloromethane (20 ml) was added to a stirred solution of the product of step b) (0.95 g, 5 mmol), (S)-3-(Acetylthio)-2-methylpropanoic acid (0.81 g, 5 mmol) and 4-(dimethylamino)pyridine (0.06 g, 0.5 mmol) in dichloromethane (30 ml). The mixture was stirred overnight, filtered and the solvent evaporated. The residue was dissolved in ethyl acetate, filtered and washed with potassium hydrogen sulphate solution, sodium bicarbonate solution and brine and the solvent evaporated. Chromatography on silica with ethyl acetate/petroleum ether as eluant gave the sub-title compound (1.1 g).

後処理

  1. filtrationfiltered
  2. customthe solvent evaporated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. filtrationfiltered
  5. washwashed with potassium hydrogen sulphate solution, sodium bicarbonate solution and brine
  6. customthe solvent evaporated

出典と根拠

ORDレコード
ord-8b1b3af61f6b4e1c9f3c3e7d4ac9d1ba
出典データセット
uspto-grants-1994_09
特許番号
US05348978

反応ノート

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