1,4-Dioxane hydrochloride → 1-Cyclopropyl-2,2-difluoroethanaminium chloride
反応式
[CH:1]1([CH:4]([NH:8]S(C(C)(C)C)=O)[CH:5]([F:7])[F:6])[CH2:3][CH2:2]1.[ClH:15].O1CCOCC1>CO>[Cl-:15].[CH:1]1([CH:4]([NH3+:8])[CH:5]([F:7])[F:6])[CH2:3][CH2:2]1参加物
4
実験手順
To a solution of N-(1-cyclopropyl-2,2-difluoroethyl)-2-methylpropane-2-sulfinamide (2.8 g, 12.4 mol) in MeOH (150 mL) was added dropwise 4 M HCl/dioxane (18.6 mL, 74.4 mmol). The mixture was stirred at room temperature overnight. The reaction mixture was concentrated under vacuum, and the solid was washed with Et2O, and dried to afford the title compound. 1H NMR (400 MHz, CD3OD) δ 6.25 (t, 1H); 2.90-3.00 (m, 1H); 1.02-1.12 (m, 1H); 0.78-0.82 (m, 2H); 0.58-0.68 (m, 2H).
後処理
- concentrationThe reaction mixture was concentrated under vacuum
- washthe solid was washed with Et2O
- customdried
出典と根拠
- ORDレコード
- ord-f64cac5d7bf549688862290a23bf4f51
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08431569B2
反応ノート
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