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Formic Acid → HCID 86684747, 화합물

HRID 2401155
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HRID 2401155 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[N:32](COCC[Si](C)(C)C)[C:31]([O:41][C@H:42]3[C@H:46]4[O:47][CH2:48][C@@H:49]([OH:50])[C@H:45]4[O:44][CH2:43]3)=[N:30][C:5]2=[N:6][C:7]=1[C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH:24]=[C:23]([CH2:25][C:26]([OH:29])([CH3:28])[CH3:27])[CH:22]=[N:21]3)=[CH:16][N:15]=2)=[CH:10][CH:9]=1.C(O)=O.OS([O-])(=O)=O.[K+].[OH-].[Na+]>CS(C)=O.CO.C1COCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[NH:32][C:31]([O:41][C@H:42]3[C@H:46]4[O:47][CH2:48][C@@H:49]([OH:50])[C@H:45]4[O:44][CH2:43]3)=[N:30][C:5]2=[N:6][C:7]=1[C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[CH:18][C:17]([N:20]3[CH:24]=[C:23]([CH2:25][C:26]([OH:29])([CH3:28])[CH3:27])[CH:22]=[N:21]3)=[CH:16][N:15]=2)=[CH:10][CH:9]=1
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참가 물질

7

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HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 516920Potassium bisulfateHCID 86684748(3R,3aR,6R,6aR)-6-[6-chloro-5-[4-[5-[4-(2-hydroxy-2-methyl-propyl)pyrazol-1-yl]-2-pyridyl]phenyl]-1-(2-trimethylsilylethoxy-methyl)imidazo[4,5-b]pyridin-2-yl]oxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-3-ol

생성물 1

HCID 86684747HCID 86684747, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 22036561Dimethyl sulfoxide methanol용매

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온도
40 °C

실험 절차

A mixture of (3R,3aR,6R,6aR)-6-[6-chloro-5-[4-[5-[4-(2-hydroxy-2-methyl-propyl)pyrazol-1-yl]-2-pyridyl]phenyl]-1-(2-trimethylsilylethoxy-methyl)imidazo[4,5-b]pyridin-2-yl]oxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-3-ol (10.1 mg, 0.014 mmol), formic acid (1.0 mL, 26.1 mmol), and saturated aqueous KHSO4 (0.05 mL) was heated to 40° C. with stirring. After 16 hours, the reaction mixture was cooled to room temperature before being cooled to 0° C. in an ice bath. The pH of the reaction mixture was adjusted to pH 14 through the addition of 5 N NaOH (5.8 mL, 29.0 mmol). THF (2 mL) was added to the reaction mixture, and the reaction was removed from the ice bath and allowed to warm to room temperature. After 30 minutes, the pH of the reaction mixture was adjusted to pH 7 through the addition of 2 N HCl. The reaction mixture was partitioned between EtOAc (30 mL) and water (20 mL). The aqueous layer was extracted with EtOAc (2×20 mL). The organic layers were combined, washed with brine (1× mL), dried over MgSO4, filtered, and evaporated under reduced pressure to give a white residue. This material was dissolved in DMSO/MeOH, and purified by HPLC reverse phase (C-18), using a 30×150 mm Sunfire™ column and eluting with a 20%-100% acetonitrile/water+0.05% TFA gradient followed by a 100% acetonitrile+0.05% TFA flush. The desired fractions were combined, evaporated under reduced pressure, and lyophilized from ethanol and benzene to afford the title compound as a pale yellow solid. LC-MS: calculated for C30H29ClN6O5 589.19 observed m/e: 589.28 (M+H)+ (Rt 1.10/2 min); 1H NMR δ (ppm) (CD3OD): 9.15 (d, J=2.5 Hz, 1H), 8.46 (dd, J=2.7 Hz, 8.9 Hz, 1H), 8.26 (s, 1H), 8.19 (d, J=8.7 Hz, 1H), 8.14 (d, J=8.4 Hz, 2H), 7.97 (s, 1H), 7.86 (d, J=8.4 Hz, 1H), 7.73 (s, 1H), 5.58 (qt, J=5.2 Hz, 1H), 4.98 (t, J=5.2 Hz, 11H), 4.47 (t, J=5.0 Hz, 1H), 4.27-4.31 (m, 1H), 4.17 (dd, J=5.4 Hz, 10.2 Hz, 1H), 4.14 (dd, J=4.7 Hz, 10.2 Hz, 1H), 3.91 (m, 1H), 3.60 (t, J=8.6 Hz, 1H), 2.73 (s, 2H), 1.25 (s, 6H).

후처리

  1. temperaturethe reaction mixture was cooled to room temperature
  2. temperaturebefore being cooled to 0° C. in an ice bath
  3. customthe reaction was removed from the ice bath
  4. temperatureto warm to room temperature
  5. waitAfter 30 minutes
  6. additionthe pH of the reaction mixture was adjusted to pH 7 through the addition of 2 N HCl
  7. customThe reaction mixture was partitioned between EtOAc (30 mL) and water (20 mL)
  8. extractionThe aqueous layer was extracted with EtOAc (2×20 mL)
  9. washwashed with brine (1× mL)
  10. dry with materialdried over MgSO4
  11. filtrationfiltered
  12. customevaporated under reduced pressure
  13. customto give a white residue
  14. custompurified by HPLC reverse phase (C-18)
  15. washeluting with a 20%-100% acetonitrile/water+0.05% TFA
  16. customflush
  17. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d115f56991694bfcb342557db1ec2bca
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796258B2

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