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Dimethylformamide → HCID 89875881, 화합물

HRID 1048634
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HRID 1048634 반응식
[CH3:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][CH:5]=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[NH:14][N:13]=[N:12]1.[C:17](=O)([O-])[O-].[K+].[K+].CN(C)C=O.S(OC)(OC)(=O)=O>O>[CH3:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][CH:5]=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[N:14]([CH3:17])[N:13]=[N:12]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 136646183HCID 136646183, 화합물

생성물 1

HCID 89875881HCID 89875881, 화합물수율 92.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Under ice-cooling, to a mixture of 1-(2-methyl-3-ethoxyphenyl)-1,4-dihydrotetrazole-5-one 39.0 g, potassium carbonate 36.7 g and N,N-dimethylformamide 400 mL was added dimethyl sulfate 44.7 g and the resulting mixtures were raised to room temperature and were stirred for seven hours. Thereto was added water and the mixtures were extracted with ethyl acetate and the organic layers were washed with 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-ethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 38.2 g.

후처리

  1. extractionthe mixtures were extracted with ethyl acetate
  2. washthe organic layers were washed with water and saturated saline
  3. dry with materialwere dried over anhydrous magnesium sulfate
  4. concentrationwere then concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8d0888b8740646e186ceb30047fdf103
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09380782B2

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