Potassium sodium tartarate → HCID 86596349, compound

HRID 1272111Notes

Reaction equation

HRID 1272111 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[N:9]=[C:10]2[C:18](=[CH:19][C:20]=1[CH3:21])[CH:17]=[C:16]1[N:11]2[C@H:12]([CH3:23])[CH2:13][NH:14][C:15]1=O.C(C(C(C([O-])=O)O)O)([O-])=O.[K+].[Na+]>COC(C)(C)C>[Cl:7][C:8]1[N:9]=[C:10]2[C:18](=[CH:19][C:20]=1[CH3:21])[CH:17]=[C:16]1[N:11]2[C@H:12]([CH3:23])[CH2:13][NH:14][CH2:15]1

Participants

5

Reactant 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 86596350HCID 86596350, compound

Product 1

HCID 86596349HCID 86596349, compound

Reagents, catalysts & solvents 1

HCID 15413tert-Butyl methyl etherSolvent

Procedure

To a stirred suspension of 5 mL tert-butyl methyl ether and 0.14 g (3.68 mmol) lithium aluminium hydride was added 0.23 g (0.92 mmol) (R)-6-chloro-4,7-dimethyl-3,4-dihydro-2H-2,4a,5-triaza-fluoren-1-one. The suspension was stirred under reflux for 15 min and, after cooling to room temperature, was poured into saturated aqueous sodium potassium tartrate solution and extracted with ethyl acetate. After filtration over speedex the phases were separated and the aqueous phase was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate and evaporated. The so-obtained product was used without further purification.

Workup

  1. temperatureunder reflux for 15 min
  2. extractionextracted with ethyl acetate
  3. filtrationAfter filtration over speedex the phases
  4. customwere separated
  5. extractionthe aqueous phase was extracted twice with ethyl acetate
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried over magnesium sulfate
  8. customevaporated
  9. customThe so-obtained product was used without further purification

Sources & evidence

ORD record
ord-650fddfa47e74d4fb356d9324a5eea60
Source dataset
uspto-grants-2007_04
Patent number
US07208494B2

Reaction notes

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