Diisopropylethylamine → HCID 67902445、化合物

HRID 232203ノート

反応式

HRID 232203 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.C(N(C(C)C)CC)(C)C.Cl[C:28]1([C:34]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][C:41]([N+:44]([O-:46])=[O:45])=[CH:40][CH:39]=2)=[O:35])[CH2:32][CH2:31][C:30](=[O:33])[O:29]1>ClCCl>[CH2:1]([O:8][C:9]([NH:11][C@@H:12]1[CH2:16][O:15][N:14]([C:28]2([C:34]([O:36][CH2:37][C:38]3[CH:43]=[CH:42][C:41]([N+:44]([O-:46])=[O:45])=[CH:40][CH:39]=3)=[O:35])[CH2:32][CH2:31][C:30](=[O:33])[O:29]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

5

反応物 3

HCID 81531DiisopropylethylamineHCID 14049831HCID 14049831、化合物HCID 14181639HCID 14181639、化合物

生成物 1

HCID 67902445HCID 67902445、化合物収率 56%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 4 ml of dichloromethane was dissolved 60 mg of (4R)-4-benzyloxycarbonylamino-3-isoxazolidinone. To the solution were added under ice-cooling 0.08 ml of diisopropyl ethylamine and 90 mg of the Compound (15) obtained in Example 15. The mixture was stirred for 15 minutes under ice-cooling, followed by stirring at room temperature for 30 minutes. The reaction solution was washed with water, which was dried (Na2SO4), then the solvent was evaporated off. The residue was subjected to a silica gel column chromatography, followed by elution with hexane-ethyl acetate (1:1) to give 71 mg of the subject Compound (8) as colorless foamy product. The IR and NMR spectra of this product were in agreement with those of the Compound (8) obtained in Example 8.

後処理

  1. additionTo the solution were added under ice-
  2. temperaturecooling
  3. stirringby stirring at room temperature for 30 minutes
  4. washThe reaction solution was washed with water, which
  5. dry with materialwas dried (Na2SO4)
  6. customthe solvent was evaporated off
  7. washfollowed by elution with hexane-ethyl acetate (1:1)

出典と根拠

ORDレコード
ord-3ac6b1211123457289d1d38d4b568b62
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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