Methanol → Methyl-7-sulfamoyl-1,4-benzodioxane-5-carboxylate

HRID 127396노트

반응식

HRID 127396 반응식
S(=O)(=O)(O)O.[S:6]([C:10]1[CH:11]=[C:12]([C:20]([OH:22])=[O:21])[C:13]2[O:18][CH2:17][CH2:16][O:15][C:14]=2[CH:19]=1)(=[O:9])(=[O:8])[NH2:7].[CH3:23]O>>[CH3:23][O:21][C:20]([C:12]1[C:13]2[O:18][CH2:17][CH2:16][O:15][C:14]=2[CH:19]=[C:10]([S:6](=[O:8])(=[O:9])[NH2:7])[CH:11]=1)=[O:22]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 205447607-Sulfamoyl-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid

생성물 1

HCID 20544687Methyl-7-sulfamoyl-1,4-benzodioxane-5-carboxylate수율 81.2%

실험 절차

429 g of methanol were introduced into a balloon flask provided with a condenser and then, under cooling, 54 g of 93% sulfuric acid and 111 g of 7-sulfamoyl-1,4-benzodioxane-5-carboxylic acid were added. The mixture was heated under reflux and then cooled. The crystals were dried off, washed with methanol and then treated with 500 cm3 of water and 5 g of sodium carbonate. The precipitate was dried off, washed with water and dried. 95 g of methyl-7-sulfamoyl-1,4-benzodioxane-5-carboxylate were obtained (M.P.: 225°-226° C.; yield: 81%).

후처리

  1. customprovided with a condenser
  2. temperatureunder cooling
  3. temperatureThe mixture was heated
  4. temperatureunder reflux
  5. temperaturecooled
  6. customThe crystals were dried off
  7. washwashed with methanol
  8. additiontreated with 500 cm3 of water and 5 g of sodium carbonate
  9. customThe precipitate was dried off
  10. washwashed with water
  11. customdried

출처 및 근거

ORD 기록
ord-2b95bf61e7584d48ab03488005498781
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255580

반응 노트

불러오는 중…