Sodium hydride → HCID 58088458, 화합물

HRID 250208

반응식

HRID 250208 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:11]=1[NH:10][CH:9]=[CH:8]2.[H-].[Na+].[CH3:14][O:15][C:16](=[O:32])[C:17](=[CH:25][C:26]1[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=1)[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19]>CN(C=O)C>[CH3:14][O:15][C:16](=[O:32])[CH:17]([CH:25]([N:10]1[C:11]2[C:7](=[CH:6][CH:5]=[CH:4][C:3]=2[O:2][CH3:1])[CH:8]=[CH:9]1)[C:26]1[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=1)[C:18]([O:20][C:21]([CH3:23])([CH3:24])[CH3:22])=[O:19]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 766607-Methoxy-1H-indoleHCID 67267624HCID 67267624, 화합물

생성물 1

HCID 58088458HCID 58088458, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 7-methoxyindole in DMF was added sodium hydride (0.086 g, 60% in oil) at 0° C. and the resulting mixture was stirred for 30 minutes. 2-Pyridin-3-ylmethylene-malonic acid tert-butyl ester methyl ester (0.470 g) was added and the mixture was stirred for 2 hours at room temperature. The reaction mixture was partitioned between ethyl acetate and water, the organic layer was washed twice with water and once with brine, then dried over magnesium sulfate, filtered and evaporated to dryness to afford the crude 2-[(7-methoxy-indol-1-yl)-pyridin-3-yl-methyl]-malonic acid tert-butyl ester methyl ester, which was crystallized from a hexane-ether mixture (0.207 g).

후처리

  1. stirringthe mixture was stirred for 2 hours at room temperature
  2. customThe reaction mixture was partitioned between ethyl acetate and water
  3. washthe organic layer was washed twice with water and once with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-f80701b00d3442db9f09c35f9d240327
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863305B2

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