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

HRID 27446

反応式

HRID 27446 の反応式
[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

参加物

4

反応物 2

HCID 119062-Chlorobenzyl chlorideHCID 31268Pyrrolidine

生成物 1

HCID 4094341-(2-Chlorobenzyl)pyrrolidine収率 75.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03cbffd768e0474ab07b13ac4c1b5e32
出典データセット
uspto-grants-1980_09
特許番号
US04221805

関連ノート

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