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

HRID 2255376ノート

反応式

HRID 2255376 の反応式
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

参加物

5

反応物 3

HCID 6212Chloroform2 回HCID 24386Thionyl ChlorideHCID 197380294-(4-Hydroxybutyl)-2,6-dimethylmorpholine

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f2ba384b21ac49138a7e7f460cba5cde
出典データセット
uspto-grants-1993_08
特許番号
US05240925

反応ノート

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