Chloroform → 4-(4-Chlorobutyl)-2,6-dimethylmorpholine hydrochloride

HRID 2255376노트

반응식

HRID 2255376 반응식
O[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH:10]([CH3:12])[O:9][CH:8]([CH3:13])[CH2:7]1.C(Cl)(Cl)[Cl:15].S(Cl)([Cl:20])=O>C(OCC)C>[ClH:15].[Cl:20][CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH:10]([CH3:12])[O:9][CH:8]([CH3:13])[CH2:7]1

참가 물질

5

반응물 3

HCID 6212Chloroform2회HCID 24386Thionyl ChlorideHCID 197380294-(4-Hydroxybutyl)-2,6-dimethylmorpholine

생성물 1

HCID 197380244-(4-Chlorobutyl)-2,6-dimethylmorpholine hydrochloride수율 85%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
40 °C

실험 절차

To a dry flask under a nitrogen atmosphere was added 0.9 g. (4.8 mmoles) of 4-(4-hydroxybutyl)-2,6-dimethylmorpholine in 2.5 ml. of chloroform. The solution was stirred and heated to 40° C. and 0.49 ml. (6.72 mmoles) of thionyl chloride in 2.5 ml. of chloroform was added slowly. The mixture was slowly heated to reflux and held for two hours, then was cooled and diluted with diethyl ether to precipitate the crude product. The crystals were filtered and washed of residual thionyl chloride using diethyl ether to obtain 1.0 g. (85% yield) of 4-(4-chlorobutyl)-2,6-dimethylmorpholine hydrochloride.

후처리

  1. additionTo a dry flask under a nitrogen atmosphere was added 0.9 g
  2. temperatureThe mixture was slowly heated
  3. temperatureto reflux
  4. temperaturewas cooled
  5. customto precipitate the crude product
  6. filtrationThe crystals were filtered
  7. washwashed of residual thionyl chloride
  8. customto obtain 1.0 g

출처 및 근거

ORD 기록
ord-f2ba384b21ac49138a7e7f460cba5cde
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05240925

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