Water → Bis(2-chloroethyl)ethylamine

HRID 517519

反応式

HRID 517519 の反応式
S(Cl)([Cl:3])=O.[CH2:5]([N:7]([CH2:11]CO)[CH2:8][CH2:9]O)[CH3:6].O.C(=O)([O-])O.[Na+].Cl[CH2:21][Cl:22]>>[Cl:3][CH2:9][CH2:8][N:7]([CH2:11][CH2:21][Cl:22])[CH2:5][CH3:6]

参加物

6

反応物 5

HCID 962WaterHCID 6344DichloromethaneHCID 8769EthyldiethanolamineHCID 24386Thionyl ChlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 10848Bis(2-chloroethyl)ethylamine収率 76%

反応条件

温度
0 °C

実験手順

24 ml (330 mmol) of thionyl chloride are added to a solution of 20 g (150 mmol) of 2-[ethyl-(2-hydroxy-ethyl)amino]ethanol in 200 ml of dichloromethane cooled to 0° C. The reaction medium is stirred at ambient temperature for 20 h. After addition of 50 ml of water then gradual addition of a saturated aqueous solution of sodium hydrogen carbonate up to a pH of 7, the reaction medium is extracted with dichloromethane. The organic phase is washed with water, dried over magnesium sulphate, filtered and concentrated under vacuum. 19.5 g (76%) of bis(2-chloroethyl)ethylamine are obtained in the form of a brown oil.

後処理

  1. extractionthe reaction medium is extracted with dichloromethane
  2. washThe organic phase is washed with water
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-3d33994b4fc84cf9933995d033aa52da
出典データセット
uspto-grants-2015_08
特許番号
US09115102B2

関連ノート

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