Sodium ethoxide → HCID 68515283, 화합물

HRID 1717427노트

반응식

HRID 1717427 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][CH:27]=[CH2:28])[CH2:20][C:21]([O:23]CC)=[O:22].[O-]CC.[Na+]>C(O)C>[CH: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])=[CH:27]\[CH3:28]

참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 14110565Ethyl 3-oxohex-5-enoateHCID 86629793HCID 86629793, 화합물

생성물 1

HCID 68515283HCID 68515283, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a solution of 4-azido-N-(2,2,2-trifluoroethyl)benzamide (2.44 g) obtained in Example 46a) in ethanol (40 ml) were added ethyl 3-oxohex-5-enoate (Tetrahedron Lett., 41, 8803-8806 (2000)) (2.10 g) synthesized separately and 20% sodium ethoxide in ethanol solution (4.6 ml), and the mixture was stirred at room temperature overnight. The solvent was evaporated under reduced pressure, and the residue was diluted with water and washed with ether. The aqueous layer was acidified with 1N hydrochloric acid, and the mixture was 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 yellow amorphous substance (1.96 g, 55%).

후처리

  1. customsynthesized separately
  2. customThe solvent was evaporated under reduced pressure
  3. additionthe residue was diluted with water
  4. washwashed with ether
  5. extractionthe mixture was extracted 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-aaaac3f4f39e4bb3a1ce955e5044c64c
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803822B2

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