Sodium hydride → HCID 68536693、化合物
反応式
[H-].[Na+].[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)=[CH:6][CH:5]=1.[C:17]([O:21][C:22](=[O:38])[CH2:23]OC1C=NC(C2C=CC=CC=2F)=CC=1)([CH3:20])([CH3:19])[CH3:18].C(OC(=O)CBr)(C)(C)C>CN(C=O)C>[C:17]([O:21][C:22](=[O:38])[CH2:23][O:16][C:13]1[CH:14]=[N:15][C:10]([C:7]2[CH:6]=[CH:5][C:4]([F:3])=[CH:9][CH:8]=2)=[CH:11][CH:12]=1)([CH3:20])([CH3:19])[CH3:18]参加物
6
実験手順
119 mg (2.72 mmol) of sodium hydride (55% in mineral oil) were added to 430 mg (2.27 mmol) of 6-(4-fluoro-phenyl)-pyridin-3-ol (prepared analogously as described in Example 76(a) to (d)) in 10 ml of DMF, and the mixture was stirred at room temperature for 60 min. Then 532 mg (2.72 mmol) of bromoacetic acid tert-butyl ester were added, and the reaction mixture was stirred at room temperature for 3 h. After evaporation, water and ethyl acetate were added. The organic phase was separated, dried, and evaporated. Yield: 433 mg.
後処理
- customprepared analogously
- stirringthe reaction mixture was stirred at room temperature for 3 h
- customAfter evaporation, water and ethyl acetate
- additionwere added
- customThe organic phase was separated
- customdried
- customevaporated
出典と根拠
- ORDレコード
- ord-fdd0f3aced614d0a8afb922b1ea14767
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08188291B2
反応ノート
読み込み中…