Phthalimide → N-Chlorophthalimide

HRID 46727

反応式

HRID 46727 の反応式
[C:1]1(=[O:11])[NH:5][C:4](=[O:6])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.O1C(CC)C1.[Cl:17]Cl>CN(C)C1C=CN=CC=1.C(Cl)Cl>[Cl:17][N:5]1[C:1](=[O:11])[C:2]2=[CH:10][CH:9]=[CH:8][CH:7]=[C:3]2[C:4]1=[O:6]

参加物

6

反応物 3

HCID 6809PhthalimideHCID 78341,2-EpoxybutaneHCID 24526Chlorine

生成物 1

HCID 18997N-Chlorophthalimide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

To 150 ml. of methylene chloride were added 7.35 g. (0.05 mole) of phthalimide, 21.5 ml. (5 equiv.) of 1,2-epoxybutane, and 0.061 g. (0.5 mmoles) of 4-dimethylaminopyridine. The mixture was cooled to 0° C. and saturated with chlorine. The resulting mixture was stirred for 20 hours at room temperature. A sample of the reaction mixture, analyzed by thin-layer chromatography (TLC), indicated that the reaction was not yet complete. The mixture was allowed to stir for an additional 24 hours, and the resulting clear yellow solution was evaporated to obtain crystalline N-chlorophthalimide. The product was vacuum dried to afford 7.7 g. (84.8%) of product. Analysis: (1) Percent Cl+ : Theory: 19.6; Found: 18.3. (2) Percent total chlorine: 18.1.

後処理

  1. stirringto stir for an additional 24 hours
  2. customthe resulting clear yellow solution was evaporated

出典と根拠

ORDレコード
ord-0dd2bcc5c80f4544942bbdab9f84b018
出典データセット
uspto-grants-1979_11
特許番号
US04175082

関連ノート

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