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

HRID 2052622

反応式

HRID 2052622 の反応式
CO.S(=O)(=O)(O)O.[CH3:8][NH:9][S:10]([C:13]1[CH:14]=[C:15]([C:23]([OH:25])=[O:24])[C:16]2[O:21][CH2:20][CH2:19][O:18][C:17]=2[CH:22]=1)(=[O:12])=[O:11].[C:26](=O)([O-])[O-].[Na+].[Na+]>O>[CH3:26][O:24][C:23]([C:15]1[C:16]2[O:21][CH2:20][CH2:19][O:18][C:17]=2[CH:22]=[C:13]([S:10](=[O:11])(=[O:12])[NH:9][CH3:8])[CH:14]=1)=[O:25]

参加物

6

反応物 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 64553172,3-Dihydro-7-(N-methylsulphamoyl)-1,4-benzodioxin-5-carboxylic acid

生成物 1

HCID 54343297Methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate収率 85%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

750 ml of methanol were introduced into a balloon flask provided with a condenser. Then, under cooling, 273 g of concentrated sulfuric acid and 160 g of 7-methylsulfamoyl-1,4-benzodioxane-5-carboxylic acid were added. The mixture was heated under reflux, cooled and poured into water and sodium carbonate. The precipitate was dried off, washed and dried. 143 g of methyl-7-methylsulfamoyl-1,4-benzodioxane-5-carboxylate were obtained (M.P.: 159°-160° C.; yield: 85%).

後処理

  1. customprovided with a condenser
  2. temperatureThen, under cooling
  3. temperatureThe mixture was heated
  4. temperatureunder reflux
  5. temperaturecooled
  6. customThe precipitate was dried off
  7. washwashed
  8. customdried

出典と根拠

ORDレコード
ord-cf47865242764896a3d20ceb75533f2e
出典データセット
uspto-grants-1980_01
特許番号
US04186135

関連ノート

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