Dimethyl Sulfate → 1-(2-Methyl-3-trifluoromethylphenyl)-4-methyl-1,4-dihydrotetrazol-5-one

HRID 1048637노트

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HRID 1048637 반응식
[CH3:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[N:12]1[C:16](=[O:17])[NH:15][N:14]=[N:13]1.[C:18](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O.C(=O)(O)[O-].[Na+]>CN(C)C=O>[CH3:1][C:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][CH:5]=[CH:4][C:3]=1[N:12]1[C:16](=[O:17])[N:15]([CH3:18])[N:14]=[N:13]1

참가 물질

6

반응물 4

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 1366461921-(2-Methyl-3-trifluoromethylphenyl)-1,4-dihydrotetrazol-5-one

생성물 1

HCID 898754051-(2-Methyl-3-trifluoromethylphenyl)-4-methyl-1,4-dihydrotetrazol-5-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
25 °C

실험 절차

A mixture of 1-(2-methyl-3-trifluoromethylphenyl)-1,4-dihydrotetrazole-5-one, potassium carbonate 11.20 g, dimethyl sulfate 3.71 g and N,N-dimethylformamide 150 mL was stirred at 25° C. for one hour. To the reaction mixtures was added aqueous saturated sodium bicarbonate solution and the mixtures were extracted with ethyl acetate. The organic layers were washed with aqueous saturated sodium bicarbonate solution and were dried over anhydrous sodium sulfate. The resulting mixtures were concentrated under reduced pressure to give 1-(2-methyl-3-trifluoromethylphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 5.13 g.

후처리

  1. customTo the reaction mixtures
  2. extractionthe mixtures were extracted with ethyl acetate
  3. washThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. dry with materialwere dried over anhydrous sodium sulfate
  5. concentrationThe resulting mixtures were concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-413944e88aa3430ea8aa7ef4a07e26e8
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09380782B2

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