1,2-Dibromoethane → 8-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic Acid

HRID 1660014

반응식

HRID 1660014 반응식
[OH:1][C:2]1[C:10]([OH:11])=[C:9]([O:12][CH3:13])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:14](Br)[CH2:15]Br>O>[CH3:13][O:12][C:9]1[C:10]2[O:11][CH2:14][CH2:15][O:1][C:2]=2[C:3]([C:4]([OH:6])=[O:5])=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 78391,2-DibromoethaneHCID 775342,3-Dihydroxy-4-methoxybenzoic acid

생성물 1

HCID 227342488-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-5-carboxylic Acid수율 57%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

171.5 g of 2,3-dihydroxy-4-methoxy benzoic acid, 515 cm3 of alcohol, 280 cm3 of soda lye and 175 g of ethylene bromide were introduced into a balloon flask provided with an agitator, a thermometer and an inlet pipe for nitrogen. The mixture was heated under reflux and then cooled and poured into 2.8 liters of water. The solution was filtered and treated with 85 cm3 of concentrated hydrochloric acid. The precipitate was dried off, washed and dried. After recrystallization in dimethylformamide, 110 g of 8-methoxy-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 224°-226° C.; yield: 57%).

후처리

  1. customprovided with an agitator
  2. temperatureThe mixture was heated
  3. temperatureunder reflux
  4. temperaturecooled
  5. filtrationThe solution was filtered
  6. additiontreated with 85 cm3 of concentrated hydrochloric acid
  7. customThe precipitate was dried off
  8. washwashed
  9. customdried
  10. customAfter recrystallization in dimethylformamide

출처 및 근거

ORD 기록
ord-b971850352f04acd9653c2cbc7cd5cc0
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04306072

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