Cyclopropylamine → HCID 43403632、化合物
反応式
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7]OS(C1C=CC(C)=CC=1)(=O)=O.[CH:19]1([NH2:22])[CH2:21][CH2:20]1>>[CH:19]1([NH:22][CH2:7][CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][O:1]2)[CH2:21][CH2:20]1参加物
3
反応条件
- 温度
- 110 °C
実験手順
A mixture of toluene-4-sulfonic acid tetrahydro-pyran-2-ylmethyl ester (500 mg, 1.85 mmol) and cyclopropylamine (2 mL, 15 mmol) is heated overnight at 110° C. in a sealed tube. The crude mixture is concentrated and taken up in CH2Cl2. Water is added, the layers are separated and the aqueous one back extracted twice with CH2Cl2. The combined organic extracts are washed with brine, dried over Na2SO4, filtered and concentrated. TLC, Rf (CH2Cl2/MeOH 95:5)=0.3, MS (LC-MS): 156.2 [M+H]+.
後処理
- concentrationThe crude mixture is concentrated
- additionWater is added
- customthe layers are separated
- extractionthe aqueous one back extracted twice with CH2Cl2
- washThe combined organic extracts are washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-495aaec245784a8d89965adb21d256c8
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07807709B2
反応ノート
読み込み中…