Hydrochloric Acid → HCID 136646185, 화합물

HRID 1048612

반응식

HRID 1048612 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[N-:5]=[N+:6]=[N-:7].[Na+].[Cl:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([N:16]=[C:17]=[O:18])[C:11]=1[CH3:19].N([O-])=O.[Na+].Cl>O.CN(C)C=O>[CH3:19][C:11]1[C:10]([Cl:9])=[CH:15][CH:14]=[CH:13][C:12]=1[N:16]1[C:17](=[O:18])[NH:7][N:6]=[N:5]1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 27357701-Chloro-3-isocyanato-2-methylbenzeneHCID 6451240Aluminum(III) ChlorideHCID 23668193Sodium Nitrite

생성물 1

HCID 136646185HCID 136646185, 화합물수율 54.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Under ice-cooling, to N,N-dimethylformamide 250 mL was added anhydrous aluminum chloride 21.9 g and the resulting mixtures were stirred for fifteen minutes. Thereto was added sodium azide 10.7 g and the resulting mixtures were stirred for fifteen minutes and thereto was then added 1-chloro-3-isocyanato-2-methylbenzene 25.0 g and the resulting mixtures were heated at 80° C. for five hours. After cooling the mixtures, to a mixture of sodium nitrite g, water 2 L and ice 500 g was added the reaction solutions with stirring. The mixtures were acidified with 10% hydrochloric acid and were extracted with ethyl acetate. The organic layers were washed with water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure to give 1-(2-methyl-3-chlorophenyl)-1,4-dihydrotetrazole-5-one 17.0 g.

후처리

  1. stirringthe resulting mixtures were stirred for fifteen minutes
  2. temperatureAfter cooling the mixtures
  3. stirringwith stirring
  4. extractionwere extracted with ethyl acetate
  5. washThe organic layers were washed with water and saturated saline
  6. dry with materialwere dried over anhydrous magnesium sulfate
  7. concentrationwere then concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6dff5a3d4def4a8e94a9f4458b88d63d
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09380782B2

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