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

HRID 979863노트

반응식

HRID 979863 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-484d99e0257c43e6aab5de40fc10ab58
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04634710

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