Ethyl 3-oxohexanoate → HCID 68517172, 화합물

HRID 1717253노트

반응식

HRID 1717253 반응식
[N:1]([C:4]1[CH:17]=[CH:16][C:7]([C:8]([NH:10][CH2:11][C:12]([F:15])([F:14])[F:13])=[O:9])=[CH:6][CH:5]=1)=[N+:2]=[N-:3].O=[C:19]([CH2:26][CH2:27][CH3:28])[CH2:20][C:21]([O:23]CC)=[O:22].[O-]CC.[Na+]>C(O)C>[CH2:26]([C:19]1[N:1]([C:4]2[CH:5]=[CH:6][C:7]([C:8]([NH:10][CH2:11][C:12]([F:14])([F:13])[F:15])=[O:9])=[CH:16][CH:17]=2)[N:2]=[N:3][C:20]=1[C:21]([OH:23])=[O:22])[CH2:27][CH3:28]

참가 물질

5

반응물 3

HCID 238498Ethyl 3-oxohexanoateHCID 2723922Sodium ethoxideHCID 86629793HCID 86629793, 화합물

생성물 1

HCID 68517172HCID 68517172, 화합물수율 100%

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
60 °C

실험 절차

To a solution of 4-azido-N-(2,2,2-trifluoroethyl)benzamide (0.98 g) obtained in Example 46a) and ethyl 3-keto-n-hexanoate (0.77 ml) in ethanol (20 ml) was added 20% sodium ethoxide in ethanol solution (1.85 ml) at room temperature, and the mixture was stirred overnight at 60° C. The reaction mixture was cooled to room temperature, and the solvent was evaporated under reduced pressure. The residue was diluted with water, and washed with ethyl acetate. The aqueous layer was acidified with 1N hydrochloric acid, and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the title compound as a pale-brown amorphous solid (1.4 g, 100%).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was diluted with water
  4. washwashed with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. dry with materialThe extract was dried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-aa34a321e21540fc8b9ac9b9f68923fb
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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