HCID 22902236, compound → HCID 22902199, compound

HRID 1489548Notes

Reaction equation

HRID 1489548 reaction equation
COC([NH:5][C:6]12[CH2:14][N:13](C(OC)=O)[CH2:12][CH:11]1[CH:10]=[CH:9][CH:8]=[CH:7]2)=O>O>[CH2:12]1[CH:11]2[C:6]([NH2:5])([CH:7]=[CH:8][CH:9]=[CH:10]2)[CH2:14][NH:13]1

Participants

3

Reactant 1

HCID 22902236HCID 22902236, compound

Product 1

HCID 22902199HCID 22902199, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

20 g of crude methyl 1-methoxycarbonylamino-8-azabicyclo[4.3.0]nona-2,4-diene-8-carboxylate are heated with 75 g (0.235 mol) of Ba(OH)2.8 H2O in 250 ml of water overnight under reflux. The BaCO3 is filtered off with suction, the filtrate is concentrated and the salt residues are boiled three times with 1,4-dioxane. The dioxane solutions are concentrated and the residue is distilled. Yield: 5 g (43.9% of theory based on Step D), boiling point: 65° C./0.2 mbar.

Workup

  1. filtrationThe BaCO3 is filtered off with suction
  2. concentrationthe filtrate is concentrated
  3. concentrationThe dioxane solutions are concentrated
  4. distillationthe residue is distilled

Sources & evidence

ORD record
ord-8bf60291ce6f49f58192a3707e6d10fc
Source dataset
uspto-grants-1997_10
Patent number
US05679689

Reaction notes

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