HCID 19814341, compound → HCID 19814236, compound

HRID 466611Notes

Reaction equation

HRID 466611 reaction equation
[CH2:1]([N:8]1[CH2:20][CH2:19][C:11]2([O:15][C:14](=[O:16])[NH:13][C:12]2(O)[CH3:17])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>O1CCOCC1>[CH2:1]([N:8]1[CH2:20][CH2:19][C:11]2([O:15][C:14](=[O:16])[NH:13][C:12]2=[CH2:17])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

3

Reactant 1

HCID 19814341HCID 19814341, compound

Product 1

HCID 19814236HCID 19814236, compoundYield 62%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

A solution containing 14.0 g of 8-benzyl-4-hydroxy-4-methyl-2-oxo-1-oxa-3,8-diazaspiro[4,5]decane in 210 ml of dioxane is boiled under nitrogen while azeotropically distilling out the water formed in the reaction. After termination of the reaction dioxane is evaporated under reduced pressure. The residue is recrystallized from ethanol under clarifying by activated carbon to give the title compound in 62% yield, m.p.: 169°-170° C.

Workup

  1. distillationwhile azeotropically distilling out the water
  2. customformed in the reaction
  3. customis evaporated under reduced pressure
  4. customThe residue is recrystallized from ethanol under clarifying by activated carbon

Sources & evidence

ORD record
ord-9bdbf9bf56ef4e0f98d6ed5b10167572
Source dataset
uspto-grants-1992_10
Patent number
US05157038

Reaction notes

Loading…