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Sodium Bicarbonate → HCID 68282650, compound

HRID 2401158
Notes
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Reaction equation

HRID 2401158 reaction equation
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[C:12]3[N:14]=[C:15]([O:25][C@H:26]4[C@H:30]5[O:31][CH2:32][C@@H:33]([OH:34])[C@H:29]5[O:28][CH2:27]4)[N:16](COCC[Si](C)(C)C)[C:11]3=[CH:10][C:9]=2[Cl:35])=[CH:4][CH:3]=1.S([O-])(O)(=O)=O.[K+].C(=O)(O)[O-].[Na+]>C(O)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[C:12]3[N:14]=[C:15]([O:25][C@H:26]4[C@H:30]5[O:31][CH2:32][C@@H:33]([OH:34])[C@H:29]5[O:28][CH2:27]4)[NH:16][C:11]3=[CH:10][C:9]=2[Cl:35])=[CH:4][CH:3]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 516892Sodium BicarbonateHCID 516920Potassium bisulfateHCID 86684749HCID 86684749, compound2×

Product 1

HCID 68282650HCID 68282650, compound

Reagents, catalysts & solvents 1

HCID 284Formic AcidSolvent

Conditions

Temperature
50 °C

Procedure

(3R,3aR,6R,6aR)-6-((5-(4-bromophenyl)-6-chloro-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazo[4,5-b]pyridin-2-yl)oxy)hexahydrofuro[3,2-b]furan-3-ol (intermediate 7, 527 mg, 0.904 mmol) was placed under nitrogen in formic acid (2.5 mL). A saturated aqueous solution of potassium hydrogen sulfate (0.4 mL) was added and the resulting mixture was allowed to stir at 50° C. for 9 hours. The mixture was cooled and added slowly to saturated aqueous sodium bicarbonate (200 mL). The mixture was extracted with ethyl acetate (2×150 mL) and concentrated under reduced pressure. The resulting white solid was dissolved in methanol (5 mL) and basified with 3N aqueous sodium hydroxide (2 mL). The mixture was stirred at room temperature for 10 minutes, then neutralized with 1N aqueous hydrochloric acid (6 mL). The mixture was poured into saturated aqueous sodium bicarbonate (25 mL) and extracted with ethyl acetate (2×50 mL). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure. The resulting white solid was chromatographed using a Biotage 25 g silica gel cartridge eluted with 0-5% methanol in dichloromethane over 20 minutes. The product fractions were combined, concentrated under reduced pressure, and dried under high vacuum to obtain a white solid. LC-MS: calculated for C18H15BrClN3O4 452.69 observed m/e: 454.02 (M+H)+ (Rt 1.84/4 min).

Workup

  1. temperatureThe mixture was cooled
  2. extractionThe mixture was extracted with ethyl acetate (2×150 mL)
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe resulting white solid was dissolved in methanol (5 mL)
  5. stirringThe mixture was stirred at room temperature for 10 minutes
  6. additionThe mixture was poured into saturated aqueous sodium bicarbonate (25 mL)
  7. extractionextracted with ethyl acetate (2×50 mL)
  8. dry with materialThe combined organic layers were dried over sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting white solid was chromatographed
  11. washeluted with 0-5% methanol in dichloromethane over 20 minutes
  12. concentrationconcentrated under reduced pressure
  13. customdried under high vacuum
  14. customto obtain a white solid
  15. custom454.02 (M+H)+ (Rt 1.84/4 min)

Sources & evidence

ORD record
ord-3d953100a58e44e2b575de9ff1cda673
Source dataset
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08796258B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes