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Methyl chloroformate → 3-(1-methoxycarbonyl-1H-tetrazol-5-yl)-4-oxo-4H-pyrido[1,2-a]pyrimidine

HRID 2259561
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HRID 2259561 반응식
[NH:1]1[C:5]([C:6]2[C:11](=[O:12])[N:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]3=[N:8][CH:7]=2)=[N:4][N:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].Cl[C:24]([O:26][CH3:27])=[O:25]>CN(C)C=O>[CH3:27][O:26][C:24]([N:1]1[C:5]([C:6]2[C:11](=[O:12])[N:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]3=[N:8][CH:7]=2)=[N:4][N:3]=[N:2]1)=[O:25]
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참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 11430Potassium CarbonateHCID 178515422HCID 178515422, 화합물

생성물 1

HCID 190014463-(1-methoxycarbonyl-1H-tetrazol-5-yl)-4-oxo-4H-pyrido[1,2-a]pyrimidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1.07 g (0.005 moles) of 3-(1H-tetrazol-5-yl)-4-oxo-4H-pyrido[1,2-a]pyrimidine; 45 ml of dimethylformamide, 0.75 g (0.0055 moles) of anhydrous potassium carbonate and 0.76 ml (0.01 moles) of methyl chloroformate was stirred at 80°-90° C. for 6 hours. The hot reaction mixture was filtered; the crystals precipitating from the filtrate were collected to obtain 0.32 g (23.5%) of the 1:1 ratio mixture of the title compounds, which on crystallization from ethanol gave the 3-(1-methoxycarbonyl-1H-tetrazol-5-yl)-4-oxo-4H-pyrido[1,2-a]pyrimidine, m.p.: 182°-183° C.

후처리

  1. filtrationThe hot reaction mixture was filtered
  2. customthe crystals precipitating from the filtrate
  3. customwere collected
  4. customto obtain
  5. customon crystallization from ethanol

출처 및 근거

ORD 기록
ord-5a1f6d7eff0548b4845fa31b53a8f1a3
출처 데이터셋
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05475000

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