HCID 89922361, 화합물 → HCID 89922320, 화합물

HRID 921897노트

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HRID 921897 반응식
[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

참가 물질

3

반응물 2

HCID 89922361HCID 89922361, 화합물HCID 178418689HCID 178418689, 화합물

생성물 1

HCID 89922320HCID 89922320, 화합물수율 12.6%

실험 절차

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,

후처리

  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

출처 및 근거

ORD 기록
ord-95b30c2d423e4c3c955641b80848e636
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273057B2

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