Diethylamine → 7-Diethylsulfamoyl-1,4-benzodioxane-5-carboxylic acid

HRID 2285491

반응식

HRID 2285491 반응식
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].C(N(CC)CC)C.Cl[S:14]([C:17]1[CH:18]=[C:19]([C:27]([OH:29])=[O:28])[C:20]2[O:25][CH2:24][CH2:23][O:22][C:21]=2[CH:26]=1)(=[O:16])=[O:15]>O>[CH2:1]([N:3]([CH2:4][CH3:5])[S:14]([C:17]1[CH:18]=[C:19]([C:27]([OH:29])=[O:28])[C:20]2[O:25][CH2:24][CH2:23][O:22][C:21]=2[CH:26]=1)(=[O:16])=[O:15])[CH3:2]

참가 물질

5

반응물 3

HCID 8021DiethylamineHCID 8471TriethylamineHCID 64553167-(Chlorosulphonyl)-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid

생성물 1

HCID 205447157-Diethylsulfamoyl-1,4-benzodioxane-5-carboxylic acid수율 74%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

200 ml of water, 100 ml of diethylamine and 200 ml of triethylamine were introduced into a balloon flask provided with an agitator and a thermometer and then 140 g of 7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were added in portions, the temperature being maintained at from 20°-30° C. The mixture was agitated at ambient temperature and then 500 ml of water were added. The solution was filtered and treated with 300 ml of hydrochloric acid. The precipitate was dried off, washed and dried. 117 g of 7-diethylsulfamoyl-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 149° C.; yield: 74%).

후처리

  1. customprovided with an agitator
  2. temperaturethe temperature being maintained at from 20°-30° C
  3. filtrationThe solution was filtered
  4. additiontreated with 300 ml of hydrochloric acid
  5. customThe precipitate was dried off
  6. washwashed
  7. customdried

출처 및 근거

ORD 기록
ord-c8e01a464187497b8069506ba675cee0
출처 데이터셋
uspto-grants-1982_04
특허 번호
US04323503

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