Bromine → 5'-Bromo-2,6-dichloro-4'-methoxy-2'-methyl-benzophenone

HRID 965463

반응식

HRID 965463 반응식
[Br:1]Br.[Cl:3][C:4]1[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[C:5]=1[C:6]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][C:9]=1[CH3:16])=[O:7].C(=O)([O-])O.[Na+]>O>[Br:1][C:12]1[C:11]([O:14][CH3:15])=[CH:10][C:9]([CH3:16])=[C:8]([C:6](=[O:7])[C:5]2[C:4]([Cl:3])=[CH:20][CH:19]=[CH:18][C:17]=2[Cl:21])[CH:13]=1

참가 물질

5

반응물 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 545052582,6-Dichloro-4'-methoxy-2'-methyl-benzophenone

생성물 1

HCID 543097645'-Bromo-2,6-dichloro-4'-methoxy-2'-methyl-benzophenone

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
20 °C

실험 절차

A solution of bromine (0.25 ml in 3 ml of trichloromethane) is added dropwise to a stirred solution of 2,6-Dichloro-4'-methoxy-2'-methyl-benzophenone (1.5 g; 5 mmol in 5 ml of trichloromethane), followed by 15 minutes of stirring at 20° C. The mixture is shaken with water, sodium hydrogencarbonate solution and water. The organic phase is dried and evaporated. The residue is purified by chromatography (flash column filled with 30 g of silicagel, elution with petrolether/ethylacetate changing from 20:1 to 9:1, 8:2, 7:3 (v/v). After evaporation, the residue crystallises when treated with petrolether/toluene to give white crystalls (0.45 g; 24% y); mp. 159° C.

후처리

  1. customThe organic phase is dried
  2. customevaporated
  3. customThe residue is purified by chromatography (flash column
  4. additionfilled with 30 g of silicagel, elution with petrolether/ethylacetate changing from 20:1 to 9:1, 8:2, 7:3 (v/v)
  5. customAfter evaporation
  6. customthe residue crystallises when
  7. additiontreated with petrolether/toluene
  8. customto give white crystalls (0.45 g; 24% y)

출처 및 근거

ORD 기록
ord-7fd439dce145453abb5a774147ffde94
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773663

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