Hydrochloric Acid → 2,6-Dichloro-4'-hydroxy-5'-nitro-2'-methyl-benzophenone

HRID 965465

反応式

HRID 965465 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][C:6]1[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[C:7]=1[C:8]([C:10]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[C:13]([O:19]C)=[CH:12][C:11]=1[CH3:21])=[O:9].Cl.O>C(Cl)Cl>[Cl:5][C:6]1[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[C:7]=1[C:8]([C:10]1[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[C:13]([OH:19])=[CH:12][C:11]=1[CH3:21])=[O:9]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 6451240Aluminum(III) ChlorideHCID 544922912,6-Dichloro-5'-nitro-4'-methoxy-2'-methyl-benzophenone

生成物 1

HCID 539076432,6-Dichloro-4'-hydroxy-5'-nitro-2'-methyl-benzophenone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
45 °C

実験手順

Aluminumchloride (1.5 g; 11 mmol) is added to a solution of 2,6-dichloro-5'-nitro-4'-methoxy-2'-methyl-benzophenone (1.8 g; 5.3 mmol) in methylenechloride (6 ml). The mixture is stirred for 30 minutes at 20° C. and for 1 hour at 45° C., 5 ml conc. hydrochloric acid/ice are added. After shaking with 20 ml of methylenechloride the organic layer is treated with 2N hydrochloric acid and with water. After drying the solvent is evaporated, the residue purified by chromatography (flash column filled with 30 g of silicagel, elution with toluene). The residue from the main fraction is treated with diisopropylether to give yellow crystalls; (1.2 g; 73% y); mp. 170° C.

後処理

  1. customAfter drying the solvent
  2. customis evaporated
  3. customthe residue purified by chromatography (flash column filled with 30 g of silicagel, elution with toluene)
  4. additionThe residue from the main fraction is treated with diisopropylether
  5. customto give yellow crystalls

出典と根拠

ORDレコード
ord-262858d7cf5046a39be6143a69e90622
出典データセット
uspto-grants-1998_06
特許番号
US05773663

関連ノート

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