Thionyl Chloride → 7-Nitro-1,4-benzodioxane-5-carbonyl chloride

HRID 1660039

반응식

HRID 1660039 반응식
S(Cl)([Cl:3])=O.[N+:5]([C:8]1[CH:9]=[C:10]([C:18]([OH:20])=O)[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=2[CH:17]=1)([O-:7])=[O:6]>CN(C)C=O>[N+:5]([C:8]1[CH:9]=[C:10]([C:18]([Cl:3])=[O:20])[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=2[CH:17]=1)([O-:7])=[O:6]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 124645337-Nitro-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid

생성물 1

HCID 205447457-Nitro-1,4-benzodioxane-5-carbonyl chloride수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

112 ml of thionyl chloride, 56 g of 7-nitro-1,4-benzodioxane-5-carboxylic acid were introduced into a 250 ml balloon flask provided with a stirrer, a thermometer and a reflux condenser. The mixture was stirred and 1 ml of dimethylformamide was added with heating. After stirring for one hour at the reflux temperature, the excess of thionyl chloride was removed by distillation under vacuum. 61 g of 7-nitro-1,4-benzodioxane-5-carbonyl chloride were obtained (M.P.: 108° C.; yield: 100%).

후처리

  1. customprovided with a stirrer
  2. temperaturewith heating
  3. stirringAfter stirring for one hour at the reflux temperature
  4. customthe excess of thionyl chloride was removed by distillation under vacuum

출처 및 근거

ORD 기록
ord-ce9ca5fa176d48f8b83c69e1998b2ee5
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04306072

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