反応式
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][N:12]=2)=[C:6]([C:21]#[N:22])[CH:5]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1.O>[OH:2][CH2:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:18])[F:19])=[CH:13][N:12]=2)=[C:6]([CH:5]=1)[C:21]#[N:22]参加物
5
反応条件
- 温度
- -55 °C
実験手順
To a solution of 3-cyano-4-(5-trifluoromethyl-pyridin-2-yloxy)-benzoic acid methyl ester (23 g, 0.070 mol) in anhydrous THF (200 mL), was added LiAlH4 (4.07 g, 0.11 mmol) portionwise at −78° C. The reaction mixture was warmed to −55° C. slowly and stirred for 20 mins, diluted with water (3 mL 0.16 mmol, slow addition), filtered and concentrated. Purification via FC (PE/EtOAc=10/1 to 5/1) afforded the title product as a colorless oil (12.5 g).
後処理
- filtrationfiltered
- concentrationconcentrated
- customPurification via FC (PE/EtOAc=10/1 to 5/1)
出典と根拠
- ORDレコード
- ord-fde3559987d24f0fb0278193cb60faaf
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09273054B2
関連ノート
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