Dichlorodiphenylmethane → 4-Bromo-7-methoxy-2,2-diphenyl-1,3-benzodioxole

HRID 2084825

반응식

HRID 2084825 반응식
[Br:1][C:2]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[C:4]([OH:5])[C:3]=1[OH:11].[C:12]1([C:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)(Cl)Cl)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)(O)[O-].[Na+]>>[Br:1][C:2]1[C:3]2[O:11][C:18]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[O:5][C:4]=2[C:6]([O:9][CH3:10])=[CH:7][CH:8]=1

참가 물질

4

반응물 3

HCID 16327DichlorodiphenylmethaneHCID 516892Sodium BicarbonateHCID 37058743-Bromo-6-methoxybenzene-1,2-diol

생성물 1

HCID 227343704-Bromo-7-methoxy-2,2-diphenyl-1,3-benzodioxole

실험 절차

3-Bromo-6-methoxycatechol (3.87 g) and diphenyl-dichloromethane (4.61 g) were heated at 170° C. with stirring without a solvent. After being allowed to stand for cooling, a saturated aqueous solution of sodium bicarbonate was added to the mixture, followed by extraction with ether. The organic layer was washed with a saturated saline and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was triturated with methanol to give Compound IIbl-a (4.7 g, 69%) as a white solid.

후처리

  1. temperaturefor cooling
  2. extractionfollowed by extraction with ether
  3. washThe organic layer was washed with a saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was triturated with methanol
  7. customto give Compound IIbl-a (4.7 g, 69%) as a white solid

출처 및 근거

ORD 기록
ord-678a91e7c7294039a4bfc238d7956dda
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716987B1

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