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

HRID 1048637ノート

反応式

HRID 1048637 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-413944e88aa3430ea8aa7ef4a07e26e8
出典データセット
uspto-grants-2016_07
特許番号
US09380782B2

反応ノート

読み込み中…