Ethyl Acetate → HCID 67902350、化合物

HRID 232226ノート

反応式

HRID 232226 の反応式
[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

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 10868DicyclohexylcarbodiimideHCID 14181640HCID 14181640、化合物HCID 679023451-(4-Nitrobenzyl) 4-methoxymethyl-2-oxoglutarate

生成物 1

HCID 67902350HCID 67902350、化合物収率 77.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c38b6ae638b3488c8958c912d8f6921a
出典データセット
uspto-grants-1989_07
特許番号
US04851422

反応ノート

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