Diethyl Ether → HCID 86678816, compound

HRID 1085032Notes

Reaction equation

HRID 1085032 reaction equation
FC(F)(F)C(O)=O.[CH3:8][N:9]([CH3:16])[C:10](=[O:15])[C@@H:11]([CH2:13][OH:14])[NH2:12].[OH-].[Na+].C(OCC)C>CO>[CH3:8][N:9]([CH3:16])[C:10](=[O:15])[C@@H:11]([CH2:13][OH:14])[NH2:12]

Participants

5

Procedure

The compound (1.00 g) prepared in Experiment 4 was dissolved in dimethylformaide (2 ml). A solution of N,N-dimethyl-D-serinamide was prepared by dissolving N,N-dimethyl-D-serinamide trifluoroacetate (590 mg) in methanol (5 ml), adding 1N-aqueous sodium hydroxide solution (2.4 ml) thereto, followed by distilling off the solvent under reduced pressure, and extracting the residue with acetonitrile (2 ml). The N,N-dimethyl-D-serinamide solution was added to the solution of the compound prepared in Experiment 4 in dimethylformamide under ice-cooling. The resulting solution was stirred for 30 minutes. The reaction solution was added to ethyl ether, and the resulting precipitates were collected by filtration to obtain yellow powder (1.1 g).

Workup

  1. dissolutionwas dissolved in dimethylformaide (2 ml)
  2. distillationby distilling off the solvent under reduced pressure
  3. extractionextracting the residue with acetonitrile (2 ml)
  4. additionThe N,N-dimethyl-D-serinamide solution was added to the solution of the compound
  5. customprepared in Experiment 4 in dimethylformamide under ice-
  6. temperaturecooling
  7. customthe resulting precipitates
  8. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-575741d8b30848548a2566205b3f5ba6
Source dataset
uspto-grants-1991_04
Patent number
US05006649

Reaction notes

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