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Dimethylformamide → HCID 89875660, 화합물

HRID 1048626
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HRID 1048626 반응식
[CH3:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][C:3]=1[N:10]1[C:14](=[O:15])[NH:13][N:12]=[N:11]1.[CH3:16]N(C)C=O.[H-].[Na+].CI>O>[CH3:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][C:3]=1[N:10]1[C:14](=[O:15])[N:13]([CH3:16])[N:12]=[N:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 136646196HCID 136646196, 화합물

생성물 1

HCID 89875660HCID 89875660, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of the above-mentioned 1-(2-methyl-3-methoxyphenyl)-1,4-dihydrotetrazole-5-one 10.00 g and N,N-dimethylformamide 100 mL was added 55% sodium hydride 2.47 g under ice-cooling. The mixtures were raised to room temperature and were stirred for one hour. To the reaction mixtures was added methyl iodide 3.5 mL under ice-cooling. The mixtures were raised to room temperature and were stirred for fourteen hours. To the reaction mixtures was added water and the mixtures were extracted with ethyl acetate. The organic layers were washed with 10% hydrochloric acid, water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-(2-methyl-3-methoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 2.19 g.

후처리

  1. temperaturecooling
  2. customTo the reaction mixtures
  3. temperaturecooling
  4. temperatureThe mixtures were raised to room temperature
  5. stirringwere stirred for fourteen hours
  6. customTo the reaction mixtures
  7. extractionthe mixtures were extracted with ethyl acetate
  8. washThe organic layers were washed with 10% hydrochloric acid, water and saturated saline
  9. dry with materialwere dried over anhydrous magnesium sulfate
  10. concentrationwere then concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-11fbc08c179f4deeb9f5e812847fab71
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09380782B2

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