Potassium Carbonate → HCID 86743156, 화합물

HRID 1904937노트

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HRID 1904937 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:11](=[O:12])[N:10]2[CH:13]=[CH:14][CH:15]=[C:16]([SH:17])[C:9]2=[N:8][CH:7]=1)=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:24]([O:28][C:29]1[CH:37]=[CH:36][C:32]([C:33](Cl)=[O:34])=[CH:31][CH:30]=1)[CH2:25][CH2:26][CH3:27]>CC(C)=O>[CH2:1]([O:3][C:4]([C:6]1[C:11](=[O:12])[N:10]2[CH:13]=[CH:14][CH:15]=[C:16]([S:17][C:33](=[O:34])[C:32]3[CH:31]=[CH:30][C:29]([O:28][CH2:24][CH2:25][CH2:26][CH3:27])=[CH:37][CH:36]=3)[C:9]2=[N:8][CH:7]=1)=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 1185614-Butoxybenzoyl chlorideHCID 143064713-ethoxycarbonyl-9-mercapto-4H-pyrido[1,2-a]pyrimidin-4-one

생성물 1

HCID 86743156HCID 86743156, 화합물수율 51.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a mixture of 0.8 g of 3-ethoxycarbonyl-9-mercapto-4H-pyrido[1,2-a]pyrimidin-4-one II-1, 0.5 g of powdery potassium carbonate and 25 ml of acetone is added 0.7 g of 4-n-butoxybenzoyl chloride with stirring, and the resultant mixture is stirred at room temperature for 2 hours. The resultant precipitate is filtered and distributed in water-chloroform. The chloroform layer is washed with saturated brine, dried over sodium sulfate and concentrated. The residue (1.1 g) is chromatographed on a column of silica gel, eluting with ethyl acetate. Concentration of the eluate affords 0.7 g of the titled compound.

후처리

  1. filtrationThe resultant precipitate is filtered
  2. washThe chloroform layer is washed with saturated brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue (1.1 g) is chromatographed on a column of silica gel
  6. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-02064b10c44d4eada0ec64f2f8f48283
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04840953

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