Dichloromethane → Bis(2-chloroethyl)ethylamine

HRID 874580

반응식

HRID 874580 반응식
S(Cl)([Cl:3])=O.[CH2:5]([N:7]([CH2:11]CO)[CH2:8][CH2:9]O)[CH3:6].C(=O)([O-])O.[Na+].Cl[CH2:20][Cl:21]>>[Cl:3][CH2:9][CH2:8][N:7]([CH2:11][CH2:20][Cl:21])[CH2:5][CH3:6]

참가 물질

5

반응물 4

HCID 6344DichloromethaneHCID 8769EthyldiethanolamineHCID 24386Thionyl ChlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 10848Bis(2-chloroethyl)ethylamine수율 76%

반응 조건

온도
0 °C

실험 절차

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

후처리

  1. extractionthe product is extracted with dichloromethane
  2. customThe organic phase obtained
  3. washis then washed with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-d5c8634a7fa0458695123b8e8108ca33
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08980897B2

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