Hydrochloric Acid → 2-Benzofuryl (2,3-dichloro-4-methoxy-phenyl) ketone

HRID 127366

反応式

HRID 127366 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][C:7]=1[O:13][CH3:14].[O:15]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[CH:17]=[C:16]1[C:24](Cl)=[O:25].Cl>C(Cl)Cl>[Cl:12][C:11]1[C:6]([Cl:5])=[C:7]([O:13][CH3:14])[CH:8]=[CH:9][C:10]=1[C:24]([C:16]1[O:15][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[CH:17]=1)=[O:25]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 161262,3-DichloroanisoleHCID 389492-Benzofurancarbonyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 545472842-Benzofuryl (2,3-dichloro-4-methoxy-phenyl) ketone収率 76.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

14 g (0.1 mole) of aluminium chloride are introduced little by little in a solution of 16 g (0.09 mole) of 2,3-dichloro-anisol and 16 g (0.09 mole) of 2-benzofurancarboxylic acid chloride in 200 ml of methylene chloride the mixture is taken up to reflux for 4 hours, then poured on crushed ice (300 g) and concentrated hydrochloric acid (10 ml); the precipitate is filtered off, washed with an aqueous solution of sodium hydroxide (10 N), then with water and dried. 22 g of 2-benzofuryl (2,3-dichloro-4-methoxy-phenyl) ketone are obtained. Melting point 148° C. after crystallization from ethylacetate.

後処理

  1. temperatureto reflux for 4 hours
  2. additionpoured
  3. filtrationthe precipitate is filtered off
  4. washwashed with an aqueous solution of sodium hydroxide (10 N)
  5. dry with materialwith water and dried

出典と根拠

ORDレコード
ord-45d108e2ff734fdfbc1b4d48fc16e452
出典データセット
uspto-grants-1981_03
特許番号
US04255585

関連ノート

読み込み中…