Water → Ethylbis(2-chloroethyl)amine

HRID 517519

반응식

HRID 517519 반응식
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]

참가 물질

6

반응물 5

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

생성물 1

HCID 10848Ethylbis(2-chloroethyl)amine수율 76%

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3d33994b4fc84cf9933995d033aa52da
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115102B2

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