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Sodium Carbonate → 6-((1R,2S)-2-Aminocyclohexylamino)-7-fluoro-4-(thiophen-2-yl)-1H-pyrrolo[3,4-c]pyridin-3(2H)-one

HRID 711592
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HRID 711592 반응식
Cl[C:2]1[C:7]2[C:8](=[O:22])[N:9](CC3C=CC(OC)=CC=3OC)[CH2:10][C:6]=2[C:5]([F:23])=[C:4]([NH:24][C@@H:25]2[CH2:30][CH2:29][CH2:28][CH2:27][C@@H:26]2[NH:31]C(=O)OC(C)(C)C)[N:3]=1.CC1(C)C(C)(C)OB([C:47]2[S:48][CH:49]=[CH:50][CH:51]=2)O1.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.O>[NH2:31][C@H:26]1[CH2:27][CH2:28][CH2:29][CH2:30][C@H:25]1[NH:24][C:4]1[N:3]=[C:2]([C:47]2[S:48][CH:49]=[CH:50][CH:51]=2)[C:7]2[C:8](=[O:22])[NH:9][CH2:10][C:6]=2[C:5]=1[F:23]
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참가 물질

6

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HCID 10340Sodium CarbonateHCID 107036284,4,5,5-Tetramethyl-2-(thiophen-2-yl)-1,3,2-dioxaborolaneHCID 86654712tert-Butyl (1S,2R)-2-(4-chloro-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)cyclohexylcarbamate

생성물 1

HCID 532511756-((1R,2S)-2-Aminocyclohexylamino)-7-fluoro-4-(thiophen-2-yl)-1H-pyrrolo[3,4-c]pyridin-3(2H)-one수율 44%

시약·촉매·용매 2

HCID 962Water용매
HCID 312751,4-Dioxane용매

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온도
80 °C

실험 절차

In a 30 mL sealed cap glass vial, tert-butyl (1S,2R)-2-(4-chloro-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)cyclohexylcarbamate (300 mg, 0.546 mmol), 4,4,5,5-tetramethyl-2-(thiophen-2-yl)-1,3,2-dioxaborolane (172 mg, 0.820 mmol), and trans-dichloro-bis(triphenylphosphine)palladium-II (38.4 mg, 0.055 mmol) were dissolved in dioxane (5 mL). An aqueous solution of 2N Na2CO3 (0.5 mL) was added, the cap was sealed, and the mixture was allowed to react at 85° C. for 3 h. The reaction mixture was subsequently diluted with water (5 mL) and extracted into EtOAc (2×30 mL). The organic layer was dried over sodium sulfate and evaporated. The resulting residue was treated with TFA (4 mL) and heated at 80° C. for 1 h to remove the protecting groups. Next, TFA was evaporated from the reaction mixture. The product was reconstituted in DMSO (8 mL) and was then purified via preparative HPLC eluting with water (0.05% TFA) and ACN (15-45% gradient, 0.035% TFA). The pure fractions were combined and evaporated to a minimal volume. Saturated aq NaHCO3 (10 mL) was added and the mixture was extracted with EtOAc (3×25 mL). The organic layers were combined, dried over sodium sulfate, and evaporated to give the title compound as a pale yellow solid (83 mg, 44%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.16-1.80 (m, 8H), 3.18 (br s, 1H), 3.86-4.11 (m, 1H), 4.39 (s, 2H), 6.60 (d, J=6.57 Hz, 1H), 7.13 (dd, J=5.05, 3.79 Hz, 1H), 7.60 (dd, J=5.18, 1.14 Hz, 1H), 8.39 (s, 1H), 9.00 (dd, J=3.79, 1.01 Hz, 1H). [M+H] calc'd for C17H19FN4OS, 347. found, 347.

후처리

  1. customIn a 30 mL sealed
  2. customthe cap was sealed
  3. customto react at 85° C. for 3 h
  4. extractionextracted into EtOAc (2×30 mL)
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customevaporated
  7. additionThe resulting residue was treated with TFA (4 mL)
  8. customto remove the protecting groups
  9. customNext, TFA was evaporated from the reaction mixture
  10. customwas then purified via preparative HPLC
  11. washeluting with water (0.05% TFA) and ACN (15-45% gradient, 0.035% TFA)
  12. customevaporated to a minimal volume
  13. additionSaturated aq NaHCO3 (10 mL) was added
  14. extractionthe mixture was extracted with EtOAc (3×25 mL)
  15. dry with materialdried over sodium sulfate
  16. customevaporated

출처 및 근거

ORD 기록
ord-36447e3a9d77446cb4dd51384d1d8b23
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181255B2

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