Sulfuric Acid → 4-(2-sulfanylidene-2,3-dihydro-1H-imidazol-1-yl)benzoic acid

HRID 64844

반응식

HRID 64844 반응식
S(=O)(=O)(O)O.[C:6]([C:11]1[CH:16]=[CH:15][C:14]([NH:17][C:18]([NH:20][CH2:21][CH:22](OCC)OCC)=[S:19])=[CH:13][CH:12]=1)([O:8]CC)=[O:7]>O>[C:6]([C:11]1[CH:12]=[CH:13][C:14]([N:17]2[CH:22]=[CH:21][NH:20][C:18]2=[S:19])=[CH:15][CH:16]=1)([OH:8])=[O:7]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 4842498N-(4-carboethoxyphenyl)-N'-(2,2-diethoxyethyl)thiourea

생성물 1

HCID 137257144-(2-sulfanylidene-2,3-dihydro-1H-imidazol-1-yl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

400 ml of 30% sulfuric acid was added to 80 g of N-(4-carboethoxyphenyl)-N'-(2,2-diethoxyethyl)thiourea, and the mixture was refluxed for 1 hour using an oil bath. The reaction mixture was cooled to room temperature, then 600 ml of water was added thereto, followed by cooling in an ice bath. Crystals precipitated were collected by filtration, then washed successively with 200 ml of water, 100 ml of isopropyl alcohol, and 100 ml of hexane. Yield: 48 g (92.8 mol%).

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureby cooling in an ice bath
  3. customCrystals precipitated
  4. filtrationwere collected by filtration
  5. washwashed successively with 200 ml of water, 100 ml of isopropyl alcohol, and 100 ml of hexane

출처 및 근거

ORD 기록
ord-5d737fca61eb4249a08d1c23ce6f277b
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04610954

연결된 노트

불러오는 중…