Hydrochloric Acid → HCID 20279442、化合物

HRID 1248353ノート

反応式

HRID 1248353 の反応式
C[O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH:9]=[C:8]([C:10]#[N:11])[C:7]=2[CH:12]=1.[Cl-].[Cl-].[Cl-].[Al+3].[Cl:17][C:18]1[CH:26]=[CH:25][CH:24]=[C:23]([Cl:27])[C:19]=1[C:20](Cl)=[O:21].Cl>ClCCl.ClC(Cl)Cl>[Cl:17][C:18]1[CH:26]=[CH:25][CH:24]=[C:23]([Cl:27])[C:19]=1[C:20]([C:4]1[C:3]([OH:2])=[CH:12][C:7]2[C:8]([C:10]#[N:11])=[CH:9][C:6]=2[CH:5]=1)=[O:21]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 783922,6-Dichlorobenzoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 21283357HCID 21283357、化合物

生成物 1

HCID 20279442HCID 20279442、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

While stirring at from 20° to 30°, 7.96 g of 5-methoxybenzocyclobutene-1-carbonitrile in 40 ml of dichloromethane are added dropwise to a suspension of 26.6 g of aluminium trichloride in 60 ml of dichloromethane. Stirring is carried out for 30 minutes at from 20° to 30° and then, over a period of 15 minutes, 20.95 g of 2,6-dichlorobenzoyl chloride are added dropwise thereto and the whole is stirred for 4 hours at room temperature and then poured into a mixture of 500 g of ice-water and 10 ml of concentrated hydrochloric acid. Stirring is then carried out for 30 minutes, 200 ml of trichloromethane are added, the whole is vigorously shaken and the organic phase is separated off, washed several times with semiconcentrated hydrochloric acid, dried over magnesium sulphate, concentrated to dryness by evaporation and recrystallised from dichloromethane/hexane. 4-(2,6-dichlorobenzoyl)-5-hydroxybenzocyclobutene-1-carbonitrile is obtained having a melting point of 174°-175°.

後処理

  1. waitover a period of 15 minutes
  2. stirringthe whole is stirred for 4 hours at room temperature
  3. stirringStirring
  4. waitis then carried out for 30 minutes
  5. stirringthe whole is vigorously shaken
  6. customthe organic phase is separated off
  7. washwashed several times with semiconcentrated hydrochloric acid
  8. dry with materialdried over magnesium sulphate
  9. concentrationconcentrated to dryness by evaporation
  10. customrecrystallised from dichloromethane/hexane

出典と根拠

ORDレコード
ord-afb67056977b48869f20e6531f90b003
出典データセット
uspto-grants-1985_06
特許番号
US04523030

反応ノート

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