Ammonium Acetate → HCID 178517437, 화합물

HRID 1414509노트

반응식

HRID 1414509 반응식
ClC(Cl)(Cl)[C:3]([NH:5][C:6]1[S:7][CH:8]=[CH:9][C:10]=1[C:11](=O)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[O:4].C([O-])(=O)C.[NH4+:25]>CS(C)=O>[C:12]1([C:11]2[C:10]3[CH:9]=[CH:8][S:7][C:6]=3[NH:5][C:3](=[O:4])[N:25]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 214877322-Trichloroacetamido-3-benzoylthiophene

생성물 1

HCID 178517437HCID 178517437, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
95 °C

실험 절차

To a solution of 2.0 g of 2-trichloroacetamido-3-benzoylthiophene in 18 ml of dimethylsulfoxide was added 0.89 g of ammonium acetate. The mixture was heated at 95° C for 2 hours, and poured into ice water, and extracted with chloroform. The chloroform layer was washed with water, dried over sodium sulfate, and the solvent was removed under reduced pressure. The residue was chromatographed on 60 g of silica gel, using methanol as an eluent to obtain 4-phenyl-1,2-dihydrothieno(2,3-d)-pyrimidin-2-one as crystals. Recrystallized from chloroform-acetone, the crystals having a melting point of 247.5°- 249° C. were obtained.

후처리

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materialdried over sodium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was chromatographed on 60 g of silica gel

출처 및 근거

ORD 기록
ord-dd6ea2bd164142d98a44efb1ba70d899
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001412

반응 노트

불러오는 중…