Diethyl Ether → 2-Chloromethyl-4-ethoxy-3,5-dimethylpyridine hydrochloride

HRID 979863ノート

反応式

HRID 979863 の反応式
[CH2:1]([O:3][C:4]1[C:9]([CH3:10])=[CH:8][N:7]=[C:6]([CH2:11]O)[C:5]=1[CH3:13])[CH3:2].S(Cl)([Cl:16])=O.CCOCC>C(Cl)Cl>[ClH:16].[Cl:16][CH2:11][C:6]1[C:5]([CH3:13])=[C:4]([O:3][CH2:1][CH3:2])[C:9]([CH3:10])=[CH:8][N:7]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 24386Thionyl ChlorideHCID 199637424-Ethoxy-3,5-dimethyl-2-pyridylmethanol

生成物 1

HCID 221514582-Chloromethyl-4-ethoxy-3,5-dimethylpyridine hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

21.0 g of 4-ethoxy-3,5-dimethyl-2-pyridylmethanol, dissolved in 110 ml of methylene chloride, were added dropwise at 0° to 10 ml of thionyl chloride in 220 ml of methylene chloride. After stirring at room temperature for 16 hours 890 ml of ether were added dropwise thereto while cooling and the mixture was stirred at room temperature for a further 2 hours. The separated crystals were filtered off under suction and washed with ether. There was obtained 2-chloromethyl-4-ethoxy-3,5-dimethylpyridine hydrochloride of melting point 156°-158°.

後処理

  1. additionwere added dropwise
  2. temperaturewhile cooling
  3. filtrationThe separated crystals were filtered off under suction
  4. washwashed with ether

出典と根拠

ORDレコード
ord-484d99e0257c43e6aab5de40fc10ab58
出典データセット
uspto-grants-1987_01
特許番号
US04634710

反応ノート

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