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

HRID 965465

반응식

HRID 965465 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
45 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-262858d7cf5046a39be6143a69e90622
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773663

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