1,1'-Carbonyldiimidazole → HCID 86714706、化合物

HRID 529221ノート

反応式

HRID 529221 の反応式
[C:1]([O:5][C:6](=[O:17])[C@H:7]([CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[NH2:8])([CH3:4])([CH3:3])[CH3:2].[C:18](N1C=CN=C1)([N:20]1[CH:24]=[CH:23][N:22]=[CH:21]1)=[O:19]>CN(C)C=O>[C:1]([O:5][C:6](=[O:17])[C@H:7]([CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[NH:8][C:18]([N:20]1[CH:24]=[CH:23][N:22]=[CH:21]1)=[O:19])([CH3:3])([CH3:4])[CH3:2]

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 7269469D-aspartic acid di-t-butyl ester

生成物 1

HCID 86714706HCID 86714706、化合物収率 70%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

L-aspartic acid di-tert-butyl ester (0.84 g, 3.0 mmol) and 1,1′-carbonyldiimidazole (2.4 g, 15 mmol) were dissolved in N,N-dimethylformamide (10 ml), and the mixture was stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added, and the mixture was washed with 1N hydrochloric acid (15 mL) and saturated brine. After drying over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (0.72 g, 2.1 mmol).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
  2. additionwas added
  3. washthe mixture was washed with 1N hydrochloric acid (15 mL) and saturated brine
  4. dry with materialAfter drying over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-f1718adaf8054d44b7648bec79cf833a
出典データセット
uspto-grants-2016_05
特許番号
US09346821B2

反応ノート

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