反応式
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([C:6]([C:12]3[N:17]=[C:16]4[C:18]([C:21]([OH:23])=O)=[CH:19][NH:20][C:15]4=[N:14][CH:13]=3)=[N:7][N:8]2[CH3:11])=[CH:4][CH:3]=1.[NH2:24][C:25]([CH3:29])([CH3:28])[C:26]#[N:27].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>[C:26]([C:25]([NH:24][C:21]([C:18]1[C:16]2=[N:17][C:12]([C:6]3[C:5]4[C:9](=[CH:10][C:2]([F:1])=[CH:3][CH:4]=4)[N:8]([CH3:11])[N:7]=3)=[CH:13][N:14]=[C:15]2[NH:20][CH:19]=1)=[O:23])([CH3:29])[CH3:28])#[N:27]参加物
6
反応物 4
HCID 81531Diisopropylethylamine
HCID 880222-Amino-2-methylpropionitrile
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 712796392-(6-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid生成物 1
試薬・触媒・溶媒 1
実験手順
A mixture of 2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[3,2-b]pyrazine-7-carboxylic acid (60 mg, 0.193 mmol), 2-amino-2-methylpropanenitrile (25 mg, 0.29 mmol), HATU (217 mg, 0.57 mmol) and DIEA (74 mg, 0.57 mmol) in DMF (3 mL) was stirred at room temperature for 16 hours. Then the mixture was filtered and the cake was washed with DMSO and MeOH to give N-(2-cyanopropan-2-yl)-2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[3,2-b]pyrazine-7-carboxamide (15 mg, 20.5%) as light yellow solid. MS: (M+H)+=400; 1H NMR (300 MHz, DMSO): δ 13.03 (s, 1H), 9.13 (s, 1H), 8.58 (s, 1H), 8.54-8.50 (m, 1H), 8.35 (s, 1H), 7.32-7.69 (m, 1H), 7.23-7.22 (m, 1H), 4.17 (s, 3H), 1.88 (s, 6H).
後処理
- filtrationThen the mixture was filtered
- washthe cake was washed with DMSO and MeOH
出典と根拠
- ORDレコード
- ord-2c7924b07bff4bfd8ddc3037af35a0cb
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
関連ノート
読み込み中…