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2-Pyrazinecarboxylic acid → HCID 44251588、化合物

HRID 2359388
ノート
印刷プレビュー

反応式

HRID 2359388 の反応式
[C:1]1([C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[C:10]([NH2:17])[CH:11]=[CH:12][CH:13]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N:18]1[CH:23]=[CH:22][N:21]=[CH:20][C:19]=1[C:24](O)=[O:25].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.CCOC(C)=O>[C:1]1([C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[C:10]([NH:17][C:24]([C:19]4[CH:20]=[N:21][CH:22]=[CH:23][N:18]=4)=[O:25])[CH:11]=[CH:12][CH:13]=3)[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10472-Pyrazinecarboxylic acidHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 199558612-Phenylquinolin-8-amine

生成物 1

HCID 44251588HCID 44251588、化合物収率 11.3%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

2-Phenylquinolin-8-amine (60 mg, 0.27 mmol) was taken up in 2 mL of DMF along with pyrazine-2-carboxylic acid (34 mg, 0.27 mmol), HATU (207 mg, 0.54 mmol) and DIEA (95 μL, 0.54 mmol). The reaction mixture was stirred at room temperature for 18 h. It was then diluted with EtOAc and washed with water. The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The resulting residue was purified by preparative HPLC (using aqueous CH3CN that has been buffered with 0.1% TFA) to afford 10 mg of the product. MS (ESI) calcd for C20H14N4O (m/z): 326.12. found: 327 [M+1].

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by preparative HPLC (using aqueous CH3CN that has been buffered with 0.1% TFA)

出典と根拠

ORDレコード
ord-0dbe8934bb77407fbf01b0aaefe415e3
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08685970B2

反応ノート

読み込み中…

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