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

HRID 127423

반응식

HRID 127423 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 blask 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 preciptate 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 preciptate was dried off
  8. washwashed
  9. customdried
  10. customAfter recrystallization in dimethylformamide

출처 및 근거

ORD 기록
ord-e4e899fafba6496286660f956febc857
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255580

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