Ammonia → 7-Sulfamoyl-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid

HRID 1413136ノート

反応式

HRID 1413136 の反応式
[NH3:1].Cl[S:3]([C:6]1[CH:7]=[C:8]([C:16]([OH:18])=[O:17])[C:9]2[O:14][CH2:13][CH2:12][O:11][C:10]=2[CH:15]=1)(=[O:5])=[O:4]>O>[S:3]([C:6]1[CH:7]=[C:8]([C:16]([OH:18])=[O:17])[C:9]2[O:14][CH2:13][CH2:12][O:11][C:10]=2[CH:15]=1)(=[O:5])(=[O:4])[NH2:1]

参加物

4

反応物 2

HCID 222AmmoniaHCID 64553167-(Chlorosulphonyl)-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid

生成物 1

HCID 205447607-Sulfamoyl-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

209 g of 34% ammonia and 97 g of 7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were introduced into a balloon flask provided with an agitator and a thermometer at a temperature of 5°-10° C. The mixture was agitated at ambient temperature and then the precipitate was dissolved in 415 cm3 of water. The solution was filtered and treated with 140 cm3 of concentrated hydrochloric acid. The crystals were dried off, washed with water and dried. 78 g of 7-sulfamoyl-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 272°-274° C.; yield: 87%).

後処理

  1. customprovided with an agitator
  2. customat a temperature of 5°-10° C
  3. filtrationThe solution was filtered
  4. additiontreated with 140 cm3 of concentrated hydrochloric acid
  5. customThe crystals were dried off
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-9cb85d3712a74d5f9c555be541ee4768
出典データセット
uspto-grants-1981_02
特許番号
US04248885

反応ノート

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