Dichloromethane → (3-Chloro-2-chloromethylpyridin-4-yl)-(2-chloroethyl)methylamine hydrochloride

HRID 1275574노트

반응식

HRID 1275574 반응식
[Cl:1][C:2]1[C:3](CO)=[N:4][CH:5]=[CH:6][C:7]=1[N:8]([CH2:10][CH2:11]O)[CH3:9].S(Cl)([Cl:17])=O.Cl[CH2:20][Cl:21]>>[ClH:1].[Cl:1][C:2]1[C:3]([CH2:20][Cl:21])=[N:4][CH:5]=[CH:6][C:7]=1[N:8]([CH2:10][CH2:11][Cl:17])[CH3:9]

참가 물질

4

반응물 3

HCID 6344Dichloromethane2회HCID 24386Thionyl ChlorideHCID 537528042-[(3-Chloro-2-hydroxymethyl-pyridin-4-yl)-methylamino]-ethanol

생성물 1

HCID 22117349(3-Chloro-2-chloromethylpyridin-4-yl)-(2-chloroethyl)methylamine hydrochloride

실험 절차

A solution of 3-chloro-4-[N-(2-hydroxyethyl)-N-methylamino]-2-hydroxymethylpyridine (2.3 g) in dichloromethane (30 ml) is treated dropwise at 0° C. with a solution of thionyl chloride (4 ml) in dichloromethane (20 ml). The temperature is then allowed to climb to 20° C. (20 min) and the temperature is then kept at 400° C. for 30 min. After stripping off the solvent in vacuo, the residue which remains is chromatographed on silica gel (petroleum ether/ethyl acetate 7/3 mixture which contains 1 ml of conc. NH3 ×aq/L). Yield: 2.6 g.

후처리

  1. customto climb to 20° C.
  2. custom(20 min)
  3. customthe residue which remains is chromatographed on silica gel (petroleum ether/ethyl acetate 7/3 mixture which contains 1 ml of conc. NH3 ×aq/L)

출처 및 근거

ORD 기록
ord-b084d3573474413cb9664f69b9e4505e
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162809

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