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Diisopropylethylamine → (S)-N-(5-(4-chlorophenyl)-6-(1,1,1-trifluoropropan-2-yloxy)pyridin-3-yl)pyridazine-3-carboxamide

HRID 1958148
ノート
印刷プレビュー

反応式

HRID 1958148 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:9])=O)[N:2]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(C(C)C)C(C)C)C.[Cl:41][C:42]1[CH:47]=[CH:46][C:45]([C:48]2[CH:49]=[C:50]([NH2:61])[CH:51]=[N:52][C:53]=2[O:54][C@@H:55]([CH3:60])[C:56]([F:59])([F:58])[F:57])=[CH:44][CH:43]=1>CN(C=O)C>[Cl:41][C:42]1[CH:43]=[CH:44][C:45]([C:48]2[CH:49]=[C:50]([NH:61][C:7]([C:3]3[N:2]=[N:1][CH:6]=[CH:5][CH:4]=3)=[O:9])[CH:51]=[N:52][C:53]=2[O:54][C@@H:55]([CH3:60])[C:56]([F:57])([F:58])[F:59])=[CH:46][CH:47]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 269369Pyridazine-3-carboxylic acidHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 672815945-(4-Chloro-phenyl)-6-((S)-2,2,2-trifluoro-1-methyl-ethoxy)-pyridin-3-ylamine

生成物 1

HCID 56961335(S)-N-(5-(4-chlorophenyl)-6-(1,1,1-trifluoropropan-2-yloxy)pyridin-3-yl)pyridazine-3-carboxamide
収率 83%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Pyridazine-3-carboxylic acid (CAN 2164-61-6; 43.1 mg, 347 μmol) was suspended in DMF (1.0 mL). TBTU (112 mg, 347 μmol), ethyldiisopropylamine (102 mg, 131 μl, 789 μmol,) and 5-(4-chloro-phenyl)-6-((S)-2,2,2-trifluoro-1-methyl-ethoxy)-pyridin-3-ylamine (0.100 g, 316 μmol) were added and the reaction mixture was stirred at room temperature for 1 h. The rection mixture was extracted with ethyl acetate and 1M citric acid solution; the organic phase was dried with MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 10 g, 10% to 50% ethyl acetate in heptane) to give 0.11 g (83%) of the title compound as white solid; MS (EI) 423.1 (M+H)+.

後処理

  1. extractionThe rection mixture was extracted with ethyl acetate and 1M citric acid solution
  2. dry with materialthe organic phase was dried with MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe crude material was purified by flash chromatography (silica gel, 10 g, 10% to 50% ethyl acetate in heptane)

出典と根拠

ORDレコード
ord-b31475174256454ca03c72527d637cbb
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08410107B2

反応ノート

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