Tetrahydrofuran → HCID 13959038, compound

HRID 255865Notes

Reaction equation

HRID 255865 reaction equation
[CH2:1]([C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[N:11]=[N:10][CH:9]=[C:8]2[C:13]([OH:15])=[O:14])[CH3:2].[CH2:16]1COCC1.C([O-])(=O)C.[Na+]>CO>[CH2:1]([C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[N:11]=[N:10][CH:9]=[C:8]2[C:13]([O:15][CH3:16])=[O:14])[CH3:2]

Participants

5

Procedure

A solution of 1.1 g of 53, 70 ml of dry THF and 0.98 g of CDII was stirred under nitrogen at room temperature until no more gas evolved (4 hours), 0.35 g of methanol and 0.03 g of sodium acetate were added and the mixture was stirred at room temperature for 3 hours. The THF was evaporated, the residue was dissolved in methylene chloride, the solution was washed with water, dried (MgSO4) and stripped of solvent. The residue was recrystallized from hexane to give 54, as a yellow solid, m.p.: 59°-60° C.

Workup

  1. additionwere added
  2. customThe THF was evaporated
  3. dissolutionthe residue was dissolved in methylene chloride
  4. washthe solution was washed with water
  5. dry with materialdried (MgSO4)
  6. customThe residue was recrystallized from hexane

Sources & evidence

ORD record
ord-036a967c0c5544aa9aa09eab923c8c90
Source dataset
uspto-grants-1987_10
Patent number
US04699651

Reaction notes

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