Pyrrolidine → 1-[4-(Chloromethyl)benzoyl]pyrrolidine

HRID 2266602ノート

反応式

HRID 2266602 の反応式
[Cl:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7](Cl)=[O:8])=[CH:5][CH:4]=1.[NH:12]1[CH2:16][CH2:15][CH2:14][CH2:13]1.C(N(C(C)C)C(C)C)C>ClCCl.Cl>[Cl:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([N:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)=[O:8])=[CH:5][CH:4]=1

参加物

6

反応物 3

HCID 31268PyrrolidineHCID 701364-(Chloromethyl)benzoyl chlorideHCID 81531Diisopropylethylamine

生成物 1

HCID 162268621-[4-(Chloromethyl)benzoyl]pyrrolidine

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 4-chloromethylbenzoyl chloride (5.0 g) and pyrrolidine (2.2 mL) in dichloromethane (30 mL) at 0° C. was treated with ethyldiisopropylamine (5.2 mL). The resulting mixture was warmed to room temperature over 1 hour and then stirred at this temperature for 2 hours. The mixture was diluted with 1.0 M aqueous hydrochloric acid, extracted with dichloromethane and the combined extracts washed with saturated aqueous sodium chloride solution and then dried over magnesium sulfate. The solvent was removed under reduced pressure to afford title compound, 6.0 g.

後処理

  1. extractionextracted with dichloromethane
  2. washthe combined extracts washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-381ce6f390064a298ea592ff8ace8898
出典データセット
uspto-grants-2010_12
特許番号
US07858640B2

反応ノート

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