Tetrahydrofuran → 2-{4-[(3-Fluoro-4-methylphenyl)oxy]phenyl}ethyl imidocarbamate
反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]([O:12][C:13]2[CH:18]=[CH:17][C:16]([CH2:19][CH2:20][OH:21])=[CH:15][CH:14]=2)=N[C:7]=1C(F)(F)F.[N:22]#[C:23][NH2:24].OS([C:29]([F:32])(F)F)(=O)=O.[CH2:33]1COCC1>>[C:23](=[NH:24])([O:21][CH2:20][CH2:19][C:16]1[CH:15]=[CH:14][C:13]([O:12][C:5]2[CH:4]=[CH:3][C:2]([CH3:7])=[C:29]([F:32])[CH:33]=2)=[CH:18][CH:17]=1)[NH2:22]参加物
5
反応条件
- 温度
- 55 °C
実験手順
To a solution of 2-(4-((5-chloro-6-(trifluoromethyl)pyridin-2-yl)oxy)phenyl)ethanol (0.2 g, 0.630 mmol) and cyanamide (0.053 g, 1.259 mmol) in dry THF (3 mL) under nitrogen was added triflic acid (0.112 mL, 1.259 mmol). The mixture was heated at 55° C. for 1 h. Purification via reverse phase flash chromatography afforded the title compound (250 mg, 0.529 mmol, 84% yield) as a white solid. LCMS: rt=2.77 min, [M+H+]=360
後処理
- customPurification via reverse phase flash chromatography
出典と根拠
- ORDレコード
- ord-dcc2a7ac65864f0b84457e29573ec0bf
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09174968B2
反応ノート
読み込み中…