Ethyl Acetate → HCID 67902350, 화합물

HRID 232226노트

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HRID 232226 반응식
[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:16][O:15][NH:14][C:13]1=[O:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:18][O:19][CH2:20][CH:21]([C:38]([O-:40])=[O:39])[CH2:22][C:23](=O)[C:24]([O:26][CH2:27][C:28]1[CH:33]=[CH:32][C:31]([N+:34]([O-:36])=[O:35])=[CH:30][CH:29]=1)=[O:25].C1CCC(N=C=NC2CCCCC2)CC1.C(OCC)(=O)C>ClCCl>[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:16][O:15][N:14]([C:23]2([C:24]([O:26][CH2:27][C:28]3[CH:29]=[CH:30][C:31]([N+:34]([O-:36])=[O:35])=[CH:32][CH:33]=3)=[O:25])[CH2:22][CH:21]([CH2:20][O:19][CH3:18])[C:38](=[O:39])[O:40]2)[C:13]1=[O:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 10868DicyclohexylcarbodiimideHCID 14181640HCID 14181640, 화합물HCID 679023451-(4-Nitrobenzyl) 4-methoxymethyl-2-oxoglutarate

생성물 1

HCID 67902350HCID 67902350, 화합물수율 77.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

In 2 ml of dichloromethane were dissolved 121 mg of (4S)-4-benzyloxycarbonylamino-3-isoxazolidinone and 200 mg of the Compound (78) obtained in Example 78. To the solution was added a solution of 137 mg of DCC in 1 ml of dichloromethane. The solution was stirred at room temperature for 2 hours. To the reaction solution was added ethyl acetate. The crystals which separated out were filtered off, and the filtrate was washed with water and dried (MgSO4). The solvent was evaporated off, and the residue was subjected to a silica gel column chromatography, followed by elution with hexane-ethyl acetate (2:1) to give 216 mg of the subject Compound (80) as a pale yellow oily product.

후처리

  1. customThe crystals which separated out
  2. filtrationwere filtered off
  3. washthe filtrate was washed with water
  4. dry with materialdried (MgSO4)
  5. customThe solvent was evaporated off
  6. washfollowed by elution with hexane-ethyl acetate (2:1)

출처 및 근거

ORD 기록
ord-c38b6ae638b3488c8958c912d8f6921a
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851422

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