Hydrochloric Acid → HCID 90229449、化合物
反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH:14]([F:16])[F:15])=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Li+].Cl>CO>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH:14]([F:15])[F:16])=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]参加物
5
実験手順
To a solution of methyl 2-chloro-5-(2,2-difluoroethoxy)benzoate (55 mg) in MeOH (1 mL) was added 1M aqueous lithium hydroxide (0.88 mL), and the solution was stirred at room temperature for 12 hours. The reaction mixture was stirred under ice-cooling, 2M hydrochloric acid was added slowly to acidify to pH 2-3, and the precipitated solid was filtered. The solid was washed sequentially with a small amount of water and diethyl ether, and dried under reduced pressure to obtain the titled compound (28 mg) as white powder.
後処理
- stirringThe reaction mixture was stirred under ice-
- temperaturecooling
- filtrationthe precipitated solid was filtered
- washThe solid was washed sequentially with a small amount of water and diethyl ether
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-1e3bc9f5b08941cf85cbca8f3529e977
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216968B2
反応ノート
読み込み中…