2-Chlorobenzyl chloride → 1-(2-Chlorobenzyl)pyrrolidine

HRID 27446

반응식

HRID 27446 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]Cl.[NH:10]1[CH2:14][CH2:13][CH2:12][CH2:11]1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][N:10]1[CH2:14][CH2:13][CH2:12][CH2:11]1

참가 물질

4

반응물 2

HCID 119062-Chlorobenzyl chlorideHCID 31268Pyrrolidine

생성물 1

HCID 4094341-(2-Chlorobenzyl)pyrrolidine수율 75.7%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of 50 g of 2-chlorobenzyl chloride in 100 ml of toluene is added in portions under agitation to a solution of 55 g of pyrrolidine in 150 ml of toluene, maintaining the temperature below 40° C. When all has been added, the mixture is brought to boiling point and heated under reflux for three hours. After cooling, it is washed twice with water, the toluene solution is dried over K2CO3, and the solvent is removed under reduced pressure. The residue is distilled under vacuum. B.P.=102°-104° C. 46 grams of N-(2-chlorobenzyl)-pyrrolidine are obtained. The analytical and spectral (I.R., N.M.R.) data agree with the proposed formula. Treating a solution in ether with gaseous HC1 gives the hydrochloride, M.P. 170° C.

후처리

  1. temperaturemaintaining the temperature below 40° C
  2. additionWhen all has been added
  3. temperatureheated
  4. temperatureunder reflux for three hours
  5. temperatureAfter cooling
  6. washit is washed twice with water
  7. dry with materialthe toluene solution is dried over K2CO3
  8. customthe solvent is removed under reduced pressure
  9. distillationThe residue is distilled under vacuum

출처 및 근거

ORD 기록
ord-03cbffd768e0474ab07b13ac4c1b5e32
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221805

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