Thionyl Chloride → (4-Chlorobutyl)dimethylamine hydrochloride

HRID 266871

반응식

HRID 266871 반응식
[CH3:1][N:2]([CH3:8])[CH2:3][CH2:4][CH2:5][CH2:6]O.S(Cl)([Cl:11])=O>C(O)C>[ClH:11].[Cl:11][CH2:6][CH2:5][CH2:4][CH2:3][N:2]([CH3:8])[CH3:1]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 833504-(Dimethylamino)butan-1-ol

생성물 1

HCID 19031551(4-Chlorobutyl)dimethylamine hydrochloride수율 170.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-(Dimethylamino)butanol (88.5g) was added dropwise at 0° C. over 2 hours to stirred thionyl chloride (93.4 g) then the mixture was stirred at ambient temperature for 1 hour and poured into ethanol (500 ml). The stirred solution was heated under reflux for 10 minutes, then the solvent was removed in vacuo. The solid residue crystallised from ethanol as a white solid which was collected by filtration, washed with ethanol, and dried in vacuo at ambient temperature for 24 hours to give 1-chloro-4-(dimethylamino)butane hydrochloride as a white solid (115 g), m.p. 100°-105° C.

후처리

  1. temperatureThe stirred solution was heated
  2. temperatureunder reflux for 10 minutes
  3. customthe solvent was removed in vacuo
  4. customThe solid residue crystallised from ethanol as a white solid which
  5. filtrationwas collected by filtration
  6. washwashed with ethanol
  7. customdried in vacuo at ambient temperature for 24 hours

출처 및 근거

ORD 기록
ord-edd142786ac549cab583847b4d40ffd5
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05652271

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