Ethyl Acetate → HCID 67902542、化合物

HRID 232222ノート

反応式

HRID 232222 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.[CH2:18]([CH:25]([C:42]([O-])=[O:43])[CH2:26][C:27](=[O:41])[C:28]([O:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([N+:38]([O-:40])=[O:39])=[CH:34][CH:33]=1)=[O:29])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.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:27]2([C:28]([O:30][CH2:31][C:32]3[CH:33]=[CH:34][C:35]([N+:38]([O-:40])=[O:39])=[CH:36][CH:37]=3)=[O:29])[CH2:26][CH:25]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:42](=[O:43])[O:41]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 67902300HCID 67902300、化合物

生成物 1

HCID 67902542HCID 67902542、化合物収率 77.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

In 6 ml of dichloromethane were dissolved 286 mg of (4S)-4-benzyloxycarbonylamino-3-isoxazolidinone and 540 mg of the Compound (73) obtained in Example 73. To the solution was added 325 mg of DCC dissolved in 2 ml of dichloromethane. The mixture was stirred at room temperature for 2 hours. To the reaction solution was added ethyl acetate, and the crystals which separated out were filtered off. The filtrate was washed with water and dried (Na2SO4), followed by evaporating off the solvent. The residue was subjected to a silica gel column chromatography, followed by elution with hexane-ethyl acetate (2:1) to give 553 mg of the subject Compound (75) 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 (Na2SO4)
  5. customby evaporating off the solvent
  6. washfollowed by elution with hexane-ethyl acetate (2:1)

出典と根拠

ORDレコード
ord-9f492b88bff34eeca0239240a779f7c9
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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