Ammonia → 5-Phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide

HRID 745808노트

반응식

HRID 745808 반응식
C([O:3][C:4]([CH:6]1[O:10][C:9]2[CH:11]=[C:12]([CH3:24])[C:13]([S:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)(=[O:17])=[O:16])=[CH:14][C:8]=2[O:7]1)=O)C.[NH3:25]>O1CCOCC1>[C:18]1([S:15]([C:13]2[C:12]([CH3:24])=[CH:11][C:9]3[O:10][CH:6]([C:4]([NH2:25])=[O:3])[O:7][C:8]=3[CH:14]=2)(=[O:17])=[O:16])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 539637605-Methyl-6-phenylsulphonyl-1,3-benzodioxole-2-carboxylic acid ethyl ester

생성물 1

HCID 543307335-Phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

34.8 g (0.1 mol) of 5-phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid ethyl ester (from Example 2) are dissolved in 350 ml of dioxan (absolute) and treated in a pressure autoclave with approximately 20 g of ammonia gas. The reaction mixture is heated for 10 hours at 80° in the autoclave, the pressure is released, and the solution is concentrated to dryness by evaporation under reduced pressure. The residue is recrystallised from 120 ml of ethanol, yielding colourless crystals of 5-phenylsulphonyl-6-methyl-1,3-benzodioxole-2-carboxylic acid amide having a melting point of 138°-141°.

후처리

  1. temperatureThe reaction mixture is heated for 10 hours at 80° in the autoclave
  2. concentrationthe solution is concentrated to dryness by evaporation under reduced pressure
  3. customThe residue is recrystallised from 120 ml of ethanol

출처 및 근거

ORD 기록
ord-034e0728bad14461940e12d8a25db720
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04600709

반응 노트

불러오는 중…