Water → HCID 18331085, 화합물

HRID 2270053노트

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HRID 2270053 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12](=[O:15])[CH2:13]Br)=[CH:8][CH:7]=1)=[O:5])[CH3:2].[N-:16]=[N+:17]=[N-:18].[Na+].O>CN(C)C=O>[N:16]([CH2:13][C:12]([C:9]1[CH:10]=[CH:11][C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])=[CH:7][CH:8]=1)=[O:15])=[N+:17]=[N-:18]

참가 물질

5

반응물 3

HCID 962WaterHCID 33557Sodium AzideHCID 11966043Ethyl 4-(2-bromoacetyl)benzoate

생성물 1

HCID 18331085HCID 18331085, 화합물수율 84.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4′-ethoxycarbonyl-2-bromoacetophenone (2.0 g) in N,N-dimethylformamide (8 ml) was added sodium azide (480 mg) at 0° C., and stirred for 2 hours at room temperature. The reaction mixture was poured into water (100 ml), extracted with diethyl ether (200 ml×2), washed with brine, and dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure. The product was purified by silica gel column chromatography (ethyl acetate:hexane=1:5) to give 2-azido-4′-ethoxycarbonylacetophenone (1.46 g).

후처리

  1. extractionextracted with diethyl ether (200 ml×2)
  2. washwashed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationMagnesium sulfate was filtered off
  5. customthe filtrate was evaporated under reduced pressure
  6. customThe product was purified by silica gel column chromatography (ethyl acetate:hexane=1:5)

출처 및 근거

ORD 기록
ord-0826fe863e664bf7a30270f5d657859b
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06331521B1

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