Sulfuric Acid → 4-Bromo-2-(2-chloro-1,1-dimethylethyl)anisole

HRID 27639

반응식

HRID 27639 반응식
[CH3:1][C:2](=[CH2:5])[CH2:3][Cl:4].[Br:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=1.S(=O)(=O)(O)O>CCOCC>[Br:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[C:9]([C:2]([CH3:5])([CH3:1])[CH2:3][Cl:4])[CH:8]=1

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 77304-BromoanisoleHCID 112413-Chloro-2-methyl-1-propene

생성물 1

HCID 46057784-Bromo-2-(2-chloro-1,1-dimethylethyl)anisole

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

2-Methylallyl chloride (108 parts) was added dropwise to a mixture of 4-bromoanisole (240 parts) and a concentrated sulphuric acid (20 parts) over a period of 2 hours at a temperature of 25°-35° C. Stirring was continued for 5 hours and the mixture was then kept for 24 hours at room temperature. Ether (400 parts) was then added and the resulting solution washed with water, aqueous sodium bicarbonate solution and water again. After drying with sodium sulphate and evaporating off the solvent the brown oil which remained was distilled yielding 4-bromo-2-(2-chloro-1,1-dimethylethyl)anisole (118 parts), boiling point 106°-120°/0.4 mm Hg. Recrystallisation from petroleum ether (b.p. 80°-100° C.) gave the pure product (98 parts), melting point 86°-88° C.

후처리

  1. waitthe mixture was then kept for 24 hours at room temperature
  2. washthe resulting solution washed with water, aqueous sodium bicarbonate solution and water again
  3. dry with materialAfter drying with sodium sulphate
  4. customevaporating off the solvent the brown oil which
  5. distillationremained was distilled

출처 및 근거

ORD 기록
ord-266fd8a62a0a47d3a939fd2dd8df2e02
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04222767

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