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Sodium Bicarbonate → HCID 178483849, compound

HRID 16686
Notes
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Reaction equation

HRID 16686 reaction equation
Cl.Cl.Cl.[Cl:4][C:5]1[CH:6]=[CH:7][C:8]([NH:11][C:12]([C:14]2[O:22][C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[C:15]=2[NH:23][C:24]([C@H:26]2[CH2:31][CH2:30][C@H:29]([NH:32][CH3:33])[CH2:28][CH2:27]2)=[O:25])=[O:13])=[N:9][CH:10]=1.[C:34]([O:38][C:39](CC(N)C=O)=[O:40])([CH3:37])([CH3:36])[CH3:35].C(OC(OCC)[CH2:50][CH2:51][NH2:52])C.[C:56](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[Cl:4][C:5]1[CH:6]=[CH:7][C:8]([NH:11][C:12]([C:14]2[O:22][C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[C:15]=2[NH:23][C:24]([C@H:26]2[CH2:31][CH2:30][C@H:29]([N:32]([CH3:56])[CH2:33][CH2:50][CH2:51][NH:52][C:39](=[O:40])[O:38][C:34]([CH3:35])([CH3:36])[CH3:37])[CH2:28][CH2:27]2)=[O:25])=[O:13])=[N:9][CH:10]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 5

HCID 516892Sodium BicarbonateHCID 5210291-Amino-3,3-diethoxypropaneHCID 5049666Sodium triacetoxyborohydrideHCID 194345963-t-Butoxycarbonyl-aminopropanalHCID 178484811HCID 178484811, compound

Product 1

HCID 178483849
HCID 178483849, compound

Reagents, catalysts & solvents 2

HCID 6212ChloroformSolventHCID 8471TriethylamineSolvent

Procedure

N-(5-Chloropyridin-2-yl)-3-({[trans-4-(methylamino)-cyclohexyl]carbonyl}amino)furo[3,2-b]pyridine-2-carboxamide trihydrochloride (300 mg) obtained in Example 119 is suspended in chloroform (7 ml). To the suspension are added 3-t-butoxycarbonyl-aminopropanal (208 mg), which can be prepared from 3-aminopropionaldehyde diethyl acetal in two steps according to the method described in a literature (Synthesis, 1994, 37) and triethylamine (334 μl) under ice-cooling, and the mixture is stirred for a few minutes. After addition of sodium triacetoxy borohydride (190 mg), the reaction solution is warmed to room temperature and stirred for 2 hours. To the reaction solution is poured saturated aqueous sodium hydrogen carbonate solution under ice-cooling, and the mixture is extracted with chloroform. The organic layer is washed successively with water and saturated brine, dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (eluent: ethyl acetate followed by ethyl acetate/methanol=20/1) to give the title compound (291 mg).

Workup

  1. temperaturecooling
  2. stirringstirred for 2 hours
  3. temperaturecooling
  4. extractionthe mixture is extracted with chloroform
  5. washThe organic layer is washed successively with water and saturated brine
  6. dry with materialdried over sodium sulfate
  7. customthe solvent is evaporated under reduced pressure
  8. customThe resulting residue is purified by NH-silica gel column chromatography (eluent: ethyl acetate followed by ethyl acetate/methanol=20/1)

Sources & evidence

ORD record
ord-ac3e7add2f9e43c8bde1cac7e0d86eba
Source dataset
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07737161B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes