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Dichloromethane → (R)-N-(4-((R)-3-aminopiperidin-1-yl)-5-fluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxypropanamide hydrochloride

HRID 875878
ノート
印刷プレビュー

反応式

HRID 875878 の反応式
F[C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]2[NH:9][CH:10]=[C:11]([NH:12][C:13](=[O:18])[C@H:14]([O:16][CH3:17])[CH3:15])[C:3]=12.[NH:19]1[CH2:24][CH2:23][CH2:22][C@@H:21]([NH:25]C(=O)OC(C)(C)C)[CH2:20]1.CCN(C(C)C)C(C)C.C(O)(C(F)(F)F)=O.C(Cl)[Cl:50]>CCCCO>[ClH:50].[NH2:25][C@@H:21]1[CH2:22][CH2:23][CH2:24][N:19]([C:2]2[C:7]([F:8])=[CH:6][N:5]=[C:4]3[NH:9][CH:10]=[C:11]([NH:12][C:13](=[O:18])[C@H:14]([O:16][CH3:17])[CH3:15])[C:3]=23)[CH2:20]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 81531DiisopropylethylamineHCID 1514172(3R)-3-Aminopiperidine, 3-BOC protectedHCID 60205634HCID 60205634、化合物

生成物 1

HCID 60205635(R)-N-(4-((R)-3-aminopiperidin-1-yl)-5-fluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxypropanamide hydrochloride
収率 93%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
140 °C

実験手順

A mixture of (R)—N-(4,5-difluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxypropanamide (0.21 g, 0.82 mmol), (R)-tert-butyl piperidin-3-ylcarbamate (0.33 g, 1.65 mmol) and DIEA (0.43 mL, 2.47 mmol) in n-BuOH (2 mL) was stirred at 140° C. (bath) for 12 hours. The solvent was removed, and the residue was dissolved in ethyl acetate (20 mL), washed with water (10 mL), brine (10 mL), dried (sodium sulfate) and concentrated in vacuo. The residue obtained was purified by reverse phase chromatography (Biotage SP4, C-18 25M+, 10-80% CH3CN/water gradient, 25 CV). The product isolated was dissolved in DCM (2 mL), and TFA (0.5 mL) was added. The mixture was stirred at room temperature for 1 hour. The solvent was removed. The residue was dissolved in DCM (1 mL) and 2N HCl in ether (3 mL) was added. The solid formed was collected to give (R)—N-(4-((R)-3-aminopiperidin-1-yl)-5-fluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxypropanamide hydrochloride (0.31 g, 93%) as a solid. 1H NMR (400 MHz, D2O) δ 8.08 (d, 1H), 7.38 (s, 1H), 4.02 (m, 1H), 3.80 (m, 1H), 3.46 (m, 2H), 3.37 (s, 3H), 3.30 (m, 1H), 3.20 (m, 1H), 2.07 (m, 1H), 1.76 (m, 1H), 1.62 (m, 2H), 1.33 (d, 3H). LCMS (APCI+) m/z 336 (M+H)+.

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in ethyl acetate (20 mL)
  3. washwashed with water (10 mL), brine (10 mL)
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated in vacuo
  6. customThe residue obtained
  7. customwas purified by reverse phase chromatography (Biotage SP4
  8. customThe product isolated
  9. stirringThe mixture was stirred at room temperature for 1 hour
  10. customThe solvent was removed
  11. dissolutionThe residue was dissolved in DCM (1 mL)
  12. addition2N HCl in ether (3 mL) was added
  13. customThe solid formed
  14. customwas collected

出典と根拠

ORDレコード
ord-c0364a904a1c44149d0dc92fcc227786
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08981085B2

反応ノート

読み込み中…

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