1,1'-Carbonyldiimidazole → HCID 86714706, 화합물

HRID 529221노트

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HRID 529221 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 86714706HCID 86714706, 화합물수율 70%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-f1718adaf8054d44b7648bec79cf833a
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346821B2

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