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

HRID 1660014

反応式

HRID 1660014 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-b971850352f04acd9653c2cbc7cd5cc0
出典データセット
uspto-grants-1981_12
特許番号
US04306072

関連ノート

読み込み中…