Thionyl Chloride → HCID 14306444, 화합물

HRID 1904938

반응식

HRID 1904938 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=O)=[CH:8][CH:7]=1)=[O:5])[CH3:2].S(Cl)(Cl)=O.[CH2:19]([O:21][C:22]([C:24]1[C:29](=[O:30])[N:28]2[CH:31]=[CH:32][CH:33]=[C:34]([SH:35])[C:27]2=[N:26][CH:25]=1)=[O:23])[CH3:20]>CN(C=O)C.C1C=CC=CC=1>[CH2:19]([O:21][C:22]([C:24]1[C:29](=[O:30])[N:28]2[CH:31]=[CH:32][CH:33]=[C:34]([S:35][C:10](=[O:12])[C:9]3[CH:8]=[CH:7][C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])=[CH:14][CH:13]=3)[C:27]2=[N:26][CH:25]=1)=[O:23])[CH3:20]

참가 물질

6

반응물 3

HCID 24386Thionyl ChlorideHCID 164720Monoethyl terephthalateHCID 143064713-ethoxycarbonyl-9-mercapto-4H-pyrido[1,2-a]pyrimidin-4-one

생성물 1

HCID 14306444HCID 14306444, 화합물수율 105.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 241Benzene용매

실험 절차

To a mixture of 1.47 g (2.4 mmol) of 4-ethoxycarbonylbenzoic acid, 3 drops of DMF and 10 ml of benzene is added 0.52 g (4.4 mmol) of thionyl chloride, and the resultant mixture is refluxed for 3 hours under stirring and concentrated in vacuo to dryness. The residue is dissolved in acetone and mixed with 1.4 g of solid potassium carbonate and then 0.5 g (2 mmol) of 3ethoxycarbonyl-9-mercapto-4H-pyrido[1,2-a]pyrimidin-4-one II-1, and the resultant mixture is vigorously stirred at room temperature for 20 minutes. The reaction mixture is concentrated in vacuo to dryness, and the residue is distributed in chloroformwater. The organic layer is dried over sodium sulfate and concentrated in vacuo. The residue is chromatographed on a column of silica gel, which is eluted with ethyl acetate to give 0.9 g of the titled compound Ie-56.

후처리

  1. concentrationconcentrated in vacuo to dryness
  2. dissolutionThe residue is dissolved in acetone
  3. additionmixed with 1.4 g of solid potassium carbonate
  4. concentrationThe reaction mixture is concentrated in vacuo to dryness
  5. dry with materialThe organic layer is dried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue is chromatographed on a column of silica gel, which
  8. washis eluted with ethyl acetate

출처 및 근거

ORD 기록
ord-f6fbb70c6e3c49548a244d6c0192a6d7
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04840953

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