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Water → 2-(6-chloro-4-fluoro-1-methylindazol-3-yl)-N-[(2R)-1-(3-cyanoazetidin-1-yl)-1-oxopropan-2-yl]-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide

HRID 246103
ノート
印刷プレビュー

反応式

HRID 246103 の反応式
[C:1]([CH:3]1[CH2:6][N:5]([C:7](=[O:42])[C@H:8]([NH:10][C:11]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[C:19]([C:22]4[C:30]5[C:25](=[CH:26][C:27]([Cl:32])=[CH:28][C:29]=5[F:31])[N:24]([CH3:33])[N:23]=4)[N:20]=3)[N:15](COCC[Si](C)(C)C)[CH:14]=2)=[O:12])[CH3:9])[CH2:4]1)#[N:2].FC(F)(F)C(O)=O.C(N)CN.O>ClCCl>[C:1]([CH:3]1[CH2:4][N:5]([C:7](=[O:42])[C@H:8]([NH:10][C:11]([C:13]2[C:21]3[C:16](=[N:17][CH:18]=[C:19]([C:22]4[C:30]5[C:25](=[CH:26][C:27]([Cl:32])=[CH:28][C:29]=5[F:31])[N:24]([CH3:33])[N:23]=4)[N:20]=3)[NH:15][CH:14]=2)=[O:12])[CH3:9])[CH2:6]1)#[N:2]
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 962WaterHCID 3301EthylenediamineHCID 6422Trifluoroacetic acidHCID 712889242-(6-Chloro-4-fluoro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [(R)-2-(3-cyano-azetidin-1-yl)-1-methyl-2-oxo-ethyl]-amide

生成物 1

HCID 71285760
2-(6-chloro-4-fluoro-1-methylindazol-3-yl)-N-[(2R)-1-(3-cyanoazetidin-1-yl)-1-oxopropan-2-yl]-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide
収率 48.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-(6-Chloro-4-fluoro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [(R)-2-(3-cyano-azetidin-1-yl)-1-methyl-2-oxo-ethyl]-amide (84 mg, 0.137 mmol) was suspended in dichloromethane (2 ml) and cooled in an ice bath. Trifluoroacetic acid (0.9 ml) was slowly added and the reaction was stirred at room temperature for 3 h then evaporated. The residue was dissolved in dichloromethane (1.4 ml) and ethylenediamine (0.55 ml, 8.25 mmol) was added. The reaction was stirred for 8 h. Water was added giving a cloudy mixture, which was extracted with ethyl acetate eight times. The combined organic layers were washed with sodium chloride solution and dried over sodium sulfate. Drying agent was filtered off and rinsed with 10% methanol/dichloromethane, and evaporated to a residue. This was combined with solid which had appeared in the aqueous layer. The combined material was purified by silica gel chromatography (methanol/dichloromethane) to give 32 mg (48%) of 2-(6-chloro-4-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [(R)-2-(3-cyano-azetidin-1-yl)-1-methyl-2-oxo-ethyl]-amide. (M+H)+=481; mp=267-268° C. 1H NMR (300 MHz, DMSO-d6) δ: 9.00 (s, 1H), 8.54 (d, J=7.2 Hz, 1H), 8.49 (d, J=10.6 Hz, 1H), 7.86-7.90 (m, 1H), 7.18 (d, J=10.2 Hz, 1H), 4.42-4.69 (m, 3H), 4.18 (s, 3H), 4.07-4.17 (m, 1H), 3.95-4.05 (m, 1H), 3.76-3.87 (m, 1H), 1.32-1.41 (m, 3H).

後処理

  1. temperaturecooled in an ice bath
  2. customthen evaporated
  3. dissolutionThe residue was dissolved in dichloromethane (1.4 ml)
  4. stirringThe reaction was stirred for 8 h
  5. customgiving a cloudy mixture, which
  6. extractionwas extracted with ethyl acetate eight times
  7. washThe combined organic layers were washed with sodium chloride solution
  8. dry with materialdried over sodium sulfate
  9. customDrying agent
  10. filtrationwas filtered off
  11. washrinsed with 10% methanol/dichloromethane
  12. customevaporated to a residue
  13. customThe combined material was purified by silica gel chromatography (methanol/dichloromethane)

出典と根拠

ORDレコード
ord-8d94e1fc66b4435ca45cc820163c608e
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658646B2

反応ノート

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