Sodium hydride → HCID 58088458、化合物

HRID 250208

反応式

HRID 250208 の反応式
[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]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 766607-Methoxy-1H-indoleHCID 67267624HCID 67267624、化合物

生成物 1

HCID 58088458HCID 58088458、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f80701b00d3442db9f09c35f9d240327
出典データセット
uspto-grants-2011_01
特許番号
US07863305B2

関連ノート

読み込み中…