Hydrochloric Acid → HCID 136646185、化合物

HRID 1048612

反応式

HRID 1048612 の反応式
[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

参加物

8

反応物 5

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

生成物 1

HCID 136646185HCID 136646185、化合物収率 54.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6dff5a3d4def4a8e94a9f4458b88d63d
出典データセット
uspto-grants-2016_07
特許番号
US09380782B2

関連ノート

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