Phosphorus pentachloride → 2-chloro-N-(2-chloroethyl)-N-methylbenzene ethanamine hydrochloride

HRID 2413110노트

반응식

HRID 2413110 반응식
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:14][CH2:15][N:16]([CH3:20])[CH2:17][CH2:18]O>C(Cl)Cl>[ClH:2].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH2:14][CH2:15][N:16]([CH2:17][CH2:18][Cl:2])[CH3:20]

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 133669692-{[2-(2-Chlorophenyl)ethyl](methyl)amino}ethan-1-ol

생성물 1

HCID 133924782-chloro-N-(2-chloroethyl)-N-methylbenzene ethanamine hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A suspension of 36 g. (0.173 mol) of phosphorous pentachloride in 300 ml. of methylene chloride was treated dropwise with a solution of 37 g. (0.173 mol) of the 2-[[2-(2-chlorophenyl)ethyl]methylamino]ethanol in 150 ml. of methylene chloride. After addition was complete, the mixture was refluxed overnight, evaporated to dryness and partitioned between dilute hydrochloric acid and ether. The aqueous layer was made basic with 10% sodium hydroxide and extracted well with ether. The ether extracts were washed with water and saturated sodium chloride, dried over magnesium sulfate and filtered. Addition of a saturated solution of ethereal hydrogen chloride gave a solid precipitate which was removed by filtration, washed with ether and dried to give 2-chloro-N-(2-chloroethyl)-N-methylbenzene ethanamine hydrochloride, m.p. 110°.

후처리

  1. additionA suspension of 36 g
  2. additionAfter addition
  3. temperaturethe mixture was refluxed overnight
  4. customevaporated to dryness
  5. custompartitioned between dilute hydrochloric acid and ether
  6. extractionextracted well with ether
  7. washThe ether extracts were washed with water and saturated sodium chloride
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. additionAddition of a saturated solution of ethereal hydrogen chloride
  11. customgave a solid precipitate which
  12. customwas removed by filtration
  13. washwashed with ether
  14. customdried

출처 및 근거

ORD 기록
ord-002e7fe81aa84e97b6cafd6b5d8cc40b
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04496558

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