Bromine → 5-Bromo-6-hydroxy-1,3-benzodioxole

HRID 2308896노트

반응식

HRID 2308896 반응식
[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][CH:5]=[C:6]([OH:10])[CH:7]=2)[O:2]1.[Br:11]Br>C(O)(=O)C>[Br:11][C:5]1[CH:4]=[C:3]2[O:2][CH2:1][O:9][C:8]2=[CH:7][C:6]=1[OH:10]

참가 물질

4

반응물 2

HCID 24408BromineHCID 68289Sesamol

생성물 1

HCID 2291485-Bromo-6-hydroxy-1,3-benzodioxole

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

To a solution of 0.18 mol (25 g) of 4,5-methylenedioxyphenol in 125 ml of glacial acetic acid, a solution of 0.16 mol (29 g) of bromine in 145 ml of glacial acetic acid is added slowly, the temperature of the reaction medium being maintained at between 15° and 25° C. When the addition is complete, the reaction medium is poured into 1.5 liters of ice-cold water. The expected product precipitates. After being drained, it is washed with water until the solvent has been removed. After being dried under vacuum in the presence of potassium hydroxide, it is recrystallized from a petroleum ether/ethyl acetate mixture or from cyclohexane. It melts at 84° C. (decomposition).

후처리

  1. temperaturethe temperature of the reaction medium being maintained at between 15° and 25° C
  2. additionWhen the addition
  3. customThe expected product precipitates
  4. washit is washed with water until the solvent
  5. customhas been removed
  6. dry with materialAfter being dried under vacuum in the presence of potassium hydroxide, it
  7. customis recrystallized from a petroleum ether/ethyl acetate mixture or from cyclohexane

출처 및 근거

ORD 기록
ord-5dae2254812e49be9a92ad83db6bb0aa
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692166

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