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Water → HCID 66976085, 화합물

HRID 1022748
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HRID 1022748 반응식
Cl[CH2:2][CH2:3][CH2:4][C:5]([NH:7][C:8]1[CH:18]=[CH:17][CH:16]=[CH:15][C:9]=1[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[O:6].[H-].[Na+].O>C1COCC1>[O:6]=[C:5]1[CH2:4][CH2:3][CH2:2][N:7]1[C:8]1[CH:18]=[CH:17][CH:16]=[CH:15][C:9]=1[C:10]([O:12][CH2:13][CH3:14])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydrideHCID 4070176HCID 4070176, 화합물

생성물 1

HCID 66976085HCID 66976085, 화합물수율 61.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 2-[(4-chlorobutanoyl)amino]benzoate (8.03 g) in THF (120 ml) was added 60% sodium hydride (2.14 g) at 0° C., and the mixture was warmed to room temperature and stirred overnight. The reaction mixture was poured into water, and the mixture was partitioned twice with ethyl acetate. The organic layers were combined, and the mixture was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (4.3 g).

후처리

  1. customthe mixture was partitioned twice with ethyl acetate
  2. washthe mixture was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-3f2832b09df741a7ac297cbb0fc78710
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722662B2

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