Potassium Carbonate → Ammonia

HRID 476560ノート

反応式

HRID 476560 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1.CS(O)(=O)=O.[Cl:21][C:22]1[CH:27]=[C:26]([Cl:28])[CH:25]=[CH:24][C:23]=1[C:29]1([CH2:32][N:33]2[CH:37]=[N:36][CH:35]=[N:34]2)[CH2:31][O:30]1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C(Cl)Cl>[NH3:3].[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]1[CH2:11][CH2:12][N:13]([CH2:31][C:29]([C:23]2[CH:24]=[CH:25][C:26]([Cl:28])=[CH:27][C:22]=2[Cl:21])([OH:30])[CH2:32][N:33]2[CH:37]=[N:36][CH:35]=[N:34]2)[CH2:14][CH2:15]1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 5921222-Piperazin-1-yl-1,3-benzothiazoleHCID 867396002-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonate

生成物 2

HCID 222AmmoniaHCID 198379583-[4-(Benzothiazol-2-yl)-piperazin-1-yl]-2-(2,4-dichlorophenyl)-1-(1H-1,2,4-triazol-1-yl)propan-2-ol

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

A mixture of benzothiazol-2-yl-piperazine (0.4 g, 1.55 mmole), 2-(2,4-dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonate (see EP-A-44605) (0.57 g, 1.55 mmole) and potassium carbonate (2 g, 14 mmole) in dioxan (20 ml) was heated at reflux for 3 days. After cooling, the mixture was diluted with methylene chloride, the insoluble inorganic material removed by filtration and the filtrate concentrated under reduced pressure. The resulting oil was purified by flash chromatography on silica gel eluting with ether (93): ethanol (7): 0.88 ammonia solution (1) to yield the desired product as a foam, m.p. 68°-85° (0.34 g, 44%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3 days
  3. temperatureAfter cooling
  4. customthe insoluble inorganic material removed by filtration
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customThe resulting oil was purified by flash chromatography on silica gel eluting with ether (93)

出典と根拠

ORDレコード
ord-15213472cb0d41cda48800d7ff4e308f
出典データセット
uspto-grants-1989_12
特許番号
US04885294

反応ノート

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