Water → Piritetrate

HRID 1583231

반응식

HRID 1583231 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([NH:9][CH3:10])[N:4]=1.C(=O)([O-])[O-].[K+].[K+].Cl[C:18]([O:20][C:21]1[CH:30]=[CH:29][C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:22]=1)=[S:19].O>CC(C)=O>[CH3:1][O:2][C:3]1[N:4]=[C:5]([N:9]([CH3:10])[C:18](=[S:19])[O:20][C:21]2[CH:30]=[CH:29][C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH:22]=2)[CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 82681O-2-Naphthyl chlorothioformateHCID 70191686-methoxy-N-methylpyridin-2-amine

생성물 1

HCID 145908Piritetrate수율 85%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

1.38 g of 2-methoxy-6-methylaminopyridine and 1.38 g of anhydrous potassium carbonate were added to 20 ml of acetone, to which 2.23 g of 2-naphthyl chlorothioformate dissolved in 20 ml of acetone was added at room temperature under stirring. The stirring was continued for 30 minutes under the same conditions and then the mixture was heated to reflux for 2 hours. The reaction mixture was poured into water after it was cooled to room temperature and the products were extracted with benzene. The benzene solution was subsequently washed with water and aqueous saturated sodium chloride solution and then benzene was removed by distillation under reduced pressure after drying over anhydrous magnesium sulfate. The residue was purified by the column chromatography (eluted with benzene on a silica gel) to give 2.75 g of O-2-naphthyl N-(6-methoxy-2-pyridyl)-N-methylthiocarbamate (Yield: 85%). A part of the product was recrystallized from acetone-hexane. Colorless crystalls having melting point of 95.5° to 97° C. were obtained.

후처리

  1. additionwas added at room temperature
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 2 hours
  4. extractionthe products were extracted with benzene
  5. washThe benzene solution was subsequently washed with water and aqueous saturated sodium chloride solution
  6. custombenzene was removed by distillation under reduced pressure
  7. dry with materialafter drying over anhydrous magnesium sulfate
  8. customThe residue was purified by the column chromatography (
  9. washeluted with benzene on a silica gel)

출처 및 근거

ORD 기록
ord-9da7a363cbf74653acec532c0012064e
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04551169

연결된 노트

불러오는 중…