HCID 89922361、化合物 → HCID 89922320、化合物

HRID 921897ノート

反応式

HRID 921897 の反応式
[C:1]([C:4]1[C:5]([Cl:28])=[C:6]([NH:12][C:13]2[N:18]=[C:17]([NH:19][CH:20]3[CH2:22][CH2:21]3)[C:16]3=[N:23][CH:24]=[C:25]([C:26]#[N:27])[N:15]3[N:14]=2)[CH:7]=[C:8]([C:10]#[N:11])[CH:9]=1)(=[O:3])[CH3:2].[CH3:29][Mg+].[Br-]>>[Cl:28][C:5]1[C:4]([C:1]([OH:3])([CH3:29])[CH3:2])=[CH:9][C:8]([C:10]#[N:11])=[CH:7][C:6]=1[NH:12][C:13]1[N:18]=[C:17]([NH:19][CH:20]2[CH2:21][CH2:22]2)[C:16]2=[N:23][CH:24]=[C:25]([C:26]#[N:27])[N:15]2[N:14]=1

参加物

3

反応物 2

HCID 89922361HCID 89922361、化合物HCID 178418689HCID 178418689、化合物

生成物 1

HCID 89922320HCID 89922320、化合物収率 12.6%

実験手順

A solution of 2-((3-acetyl-2-chloro-5-cyanophenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (Example 675) (60 mg, 0.15 mmol) in TIIF (8 mL) was cooled in an ice bath and MeMgBr (3 M in THF, 0.26 mL, 0.76 mmol) was added and the reaction was allowed to warm to room temperature. It was quenched with sat. aq. NH4Cl solution and extracted twice with EtOAc. The organic extracts were washed with brine, dried with sodium sulfate, and the solvent removed. HPLC purification afforded 7.7 mg of the title compound,

後処理

  1. customIt was quenched with sat. aq. NH4Cl solution
  2. extractionextracted twice with EtOAc
  3. washThe organic extracts were washed with brine
  4. dry with materialdried with sodium sulfate
  5. customthe solvent removed
  6. customHPLC purification

出典と根拠

ORDレコード
ord-95b30c2d423e4c3c955641b80848e636
出典データセット
uspto-grants-2016_03
特許番号
US09273057B2

反応ノート

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