Ammonium Acetate → HCID 178517437、化合物

HRID 1414509ノート

反応式

HRID 1414509 の反応式
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

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 214877322-Trichloroacetamido-3-benzoylthiophene

生成物 1

HCID 178517437HCID 178517437、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
95 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dd6ea2bd164142d98a44efb1ba70d899
出典データセット
uspto-grants-1977_01
特許番号
US04001412

反応ノート

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