Toluene → 2-(1-Chloroethyl)-4-methoxy-pyridine hydrochloride
反応式
S(Cl)([Cl:3])=O.[CH3:5][O:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([CH:13](O)[CH3:14])[CH:8]=1.C1(C)C=CC=CC=1>ClCCl>[ClH:3].[Cl:3][CH:13]([C:9]1[CH:8]=[C:7]([O:6][CH3:5])[CH:12]=[CH:11][N:10]=1)[CH3:14]参加物
5
実験手順
36 ml of thionyl chloride are added dropwise to a cooled suspension of 57 g of (±)-1-[4-methoxy-2-pyridyl]ethanol in 400 ml of dichloromethane, in such a way that the internal temperature does not exceed 15° C. The mixture is then heated under reflux for 2.5 h, treated with 300 ml of toluene and concentrated to 150 ml. The reaction product which has precipitated is filtered off with suction and rinsed with cold toluene and petroleum ether. This gives 76.4 g (98.2%) of the title compound of m.p. 113°-116° C.
後処理
- customdoes not exceed 15° C
- temperatureThe mixture is then heated
- temperatureunder reflux for 2.5 h
- concentrationconcentrated to 150 ml
- customThe reaction product which has precipitated
- filtrationis filtered off with suction
- washrinsed with cold toluene and petroleum ether
出典と根拠
- ORDレコード
- ord-d9e9a77157924c8592aec16db23141ed
- 出典データセット
- uspto-grants-1987_08
- 特許番号
- US04686230
反応ノート
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