Chlorosulfonic acid → 7-(Chlorosulphonyl)-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid

HRID 127393

반응식

HRID 127393 반응식
[Cl:1][S:2]([OH:5])(=O)=[O:3].[O:6]1[C:11]2[CH:12]=[CH:13][CH:14]=[C:15]([C:16]([OH:18])=[O:17])[C:10]=2[O:9][CH2:8][CH2:7]1>>[Cl:1][S:2]([C:13]1[CH:14]=[C:15]([C:16]([OH:18])=[O:17])[C:10]2[O:9][CH2:8][CH2:7][O:6][C:11]=2[CH:12]=1)(=[O:5])=[O:3]

참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 781842,3-Dihydro-1,4-benzodioxin-5-carboxylic acid

생성물 1

HCID 64553167-(Chlorosulphonyl)-2,3-dihydro-1,4-benzodioxin-5-carboxylic acid수율 93.5%

반응 조건

온도
55 °C

실험 절차

670 g of chlorosulfonic acid were introduced into a balloon flask provided with a condenser and a thermometer. 173 g of 1,4-benzodioxane-5-carboxylic acid were added in portions with the temperature being maintained at 5°-10° C. The mixture was heated at 55° C. and then cooled and poured into ice. The precipitate was dried off, washed and dried again. 250 g of 7-chlorosulfonyl-1,4-benzodioxane-5-carboxylic acid were obtained (M.P.: 210°-215° C.; yield: 93.5%).

후처리

  1. customprovided with a condenser
  2. temperaturebeing maintained at 5°-10° C
  3. temperaturecooled
  4. additionpoured into ice
  5. customThe precipitate was dried off
  6. washwashed
  7. customdried again

출처 및 근거

ORD 기록
ord-0bdad6f393eb40bfb277d8fb0bb16f6a
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255580

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