Dimethylformamide dimethyl acetal → 4-(4-Chlorophenoxy)-1-(dimethylamino)pent-1-en-3-one

HRID 1075541

反応式

HRID 1075541 の反応式
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]([O:6][CH:7]([CH3:11])[C:8](=[O:10])[CH3:9])=[CH:4][CH:3]=1.CO[CH:16](OC)[N:17]([CH3:19])[CH3:18]>CO>[Cl:1][C:2]1[CH:13]=[CH:12][C:5]([O:6][CH:7]([CH3:11])[C:8](=[O:10])[CH:9]=[CH:16][N:17]([CH3:19])[CH3:18])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 37226323-(4-Chlorophenoxy)-2-butanone

生成物 1

HCID 37226344-(4-Chlorophenoxy)-1-(dimethylamino)pent-1-en-3-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
120 °C

実験手順

A mixture of 3-(4-chlorophenoxy)-2-butanone (34.50 g) and N,N-dimethylformamide dimethylacetal (20.70 g) was heated under argon in an oil bath at 120° C. for 13 hours. The methanol produced in the reaction was removed under reduced pressure and the residual oil was triturated with n-hexane. The solid was collected by filtration and washed with cold diethyl ether to give 4-(4-chlorophenoxy)-1-(dimethylamino)-1-penten-3-one. Yield 32.50 g.

後処理

  1. customwas removed under reduced pressure
  2. customthe residual oil was triturated with n-hexane
  3. filtrationThe solid was collected by filtration
  4. washwashed with cold diethyl ether

出典と根拠

ORDレコード
ord-07a818f0fb74421495b63567ca34fa2a
出典データセット
uspto-grants-1999_05
特許番号
US05905079

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