Water → Tert-Butyl (2-(methylthio)ethyl)carbamate
反応式
Cl.[CH3:2][S:3][CH2:4][CH2:5][NH2:6].[CH2:7](N(CC)CC)C.[OH2:14].[C:15](OCC)(=[O:17])C.O1[CH2:25][CH2:24][CH2:23]C1>>[CH3:2][S:3][CH2:4][CH2:5][NH:6][C:15](=[O:17])[O:14][C:24]([CH3:23])([CH3:25])[CH3:7]参加物
6
実験手順
In a dried reaction flask, 2-(methylthio)ethylamine hydrochloride (6.382 g, 50.0 mmol) and TEA (triethylamine) (13.9 mL, 100 mmol) were dissolved in tetrahydrofuran (63.3 mL). To the mixture was added dropwise Boc2O(di-tert-butyl dicarbonate) (12.3 g, 56.4 mmol) dissolved in tetrahydrofuran (10 mL) under an ice-salt bath. The mixture was stirred at room temperature for 21 hr. Water and ethyl acetate were added. The mixture was extracted with ethyl acetate. The combined organic phase was washed with brine, dried over anhydrous sodium sulfate, and concentrated to produce a crude colorless oil (11.752 g).
後処理
- extractionThe mixture was extracted with ethyl acetate
- washThe combined organic phase was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-d3523f4989dd440b8145d046539256e9
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08946279B2
反応ノート
読み込み中…