Hydrochloric Acid → 2-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamine

HRID 365000노트

반응식

HRID 365000 반응식
Cl.[NH2:2][CH2:3][CH2:4][SH:5].[O-]CC.[Na+].Cl.Cl.Cl[CH2:13][C:14]1[CH:19]=[C:18]([CH2:20][N:21]([CH3:23])[CH3:22])[CH:17]=[CH:16][N:15]=1.Cl>C(O)C.O>[CH3:22][N:21]([CH2:20][C:18]1[CH:17]=[CH:16][N:15]=[C:14]([CH2:13][S:5][CH2:4][CH2:3][NH2:2])[CH:19]=1)[CH3:23]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 9082Cysteamine HydrochlorideHCID 2723922Sodium ethoxideHCID 132926032-Chloromethyl-4-dimethylaminomethylpyridine dihydrochloride

생성물 1

HCID 132773272-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamine수율 73.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

Cysteamine hydrochloride (3.75 g) was added to a stirred solution of sodium ethoxide (prepared from 2.83 g sodium) in ethanol (200 ml) and the mixture was cooled to less than 10°. 2-Chloromethyl-4-dimethylaminomethylpyridine dihydrochloride (7.3 g) was added portionwise and the solution was stirred for 1 hour. Water (200 ml) was added, the pH was adjusted to ca. 4 with hydrochloric acid and the volume was reduced to ca. 100 ml. The solution was extracted with chloroform, the aqueous phase was basified to pH 12 and extracted with chloroform to give 2-[4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine (4.7 g) as an oil.

후처리

  1. temperaturethe mixture was cooled to less than 10°
  2. extractionThe solution was extracted with chloroform
  3. extractionextracted with chloroform

출처 및 근거

ORD 기록
ord-db9cecb607904804810b09c151d26606
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04607107

반응 노트

불러오는 중…