Dicyclohexylcarbodiimide → HCID 54392109, 화합물

HRID 2226578노트

반응식

HRID 2226578 반응식
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]

참가 물질

6

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 2724506D-beta-acetylthioisobutyric acidHCID 54445895HCID 54445895, 화합물

생성물 1

HCID 54392109HCID 54392109, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8b1b3af61f6b4e1c9f3c3e7d4ac9d1ba
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05348978

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