Sodium Sulfate → (2-Amino-6-fluorophenyl)methanol
反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[NH2:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:9]=1[C:10](O)=[O:11].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[NH2:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:9]=1[CH2:10][OH:11]参加物
5
実験手順
LAH (987 mg, 26 mmol) was added slowly to a solution of 2-amino-6-fluoro-benzoic acid (2.69 g, 17.3 mmol) in dry THF (20 mL) at 0° C. The mixture was stirred at room temperature for approximately 1 hr and cooled to 0° C. again. Na2SO4. 10H2O (10 g) was added slowly with stirring for 20 minutes. The mixture was filtered, the solid was washed with THF. The solution was concentrated to yield a yellow solid as (2-amino-6-fluoro-phenyl)-methanol (2.49 g). MS [M−OH]+: 124.1; tR=0.57 min. (method 1)
後処理
- temperaturecooled to 0° C. again
- addition10H2O (10 g) was added slowly
- stirringwith stirring for 20 minutes
- filtrationThe mixture was filtered
- washthe solid was washed with THF
- concentrationThe solution was concentrated
出典と根拠
- ORDレコード
- ord-1ebad88f8c4f4acdaf6118055c1e51ed
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481738B2
反応ノート
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