Thionyl Chloride → (4-Chlorobutyl)dimethylamine hydrochloride

HRID 266871

反応式

HRID 266871 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 19031551(4-Chlorobutyl)dimethylamine hydrochloride収率 170.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-edd142786ac549cab583847b4d40ffd5
出典データセット
uspto-grants-1997_07
特許番号
US05652271

関連ノート

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