Thionyl Chloride → HCID 66853164、化合物
反応式
S(Cl)([Cl:3])=O.[N:5]1([CH2:10][C:11]2([CH2:14]O)[CH2:13][CH2:12]2)[CH2:9][CH2:8][CH2:7][CH2:6]1>C1(C)C=CC=CC=1>[ClH:3].[Cl:3][CH2:14][C:11]1([CH2:10][N:5]2[CH2:9][CH2:8][CH2:7][CH2:6]2)[CH2:13][CH2:12]1参加物
4
反応条件
- 温度
- 110 °C
実験手順
Thionyl chloride (1 mL, 13.7 mmol) was added to a solution of (1-pyrrolidin-1-ylmethyl-cyclopropyl)-methanol (1.45 g, 9.3 mmol) in toluene (20 mL) to give a pale brown suspension. The suspension was heated, 110° C., for ˜3 hrs. to give a dark brown suspension. The resulting suspension was allowed to cool and concentrated to a brown solid. Tritruation with diethyl ether (40 mL) gave the desired intermediate, 1-(1-chloromethyl-cyclopropylmethyl)-pyrrolidine hydrochloride as a brown powder 1.6 g, 82%.
後処理
- customto give a pale brown suspension
- customto give a dark brown suspension
- temperatureto cool
- concentrationconcentrated to a brown solid
出典と根拠
- ORDレコード
- ord-550ee2b99c3942b4987e4142eedaf722
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916591B2
反応ノート
読み込み中…