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

HRID 127396ノート

反応式

HRID 127396 の反応式
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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-2b95bf61e7584d48ab03488005498781
出典データセット
uspto-grants-1981_03
特許番号
US04255580

反応ノート

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