HCID 19761221, compound → HCID 19761240, compound

HRID 2082347Notes

Reaction equation

HRID 2082347 reaction equation
C([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH3:20])[C:15](=[O:19])[O:16][CH2:17][CH3:18])[CH2:10][CH2:9]1)C1C=CC=CC=1>C(O)(=O)C.[Pd]>[NH:8]1[CH2:9][CH2:10][CH:11]([N:14]([CH3:20])[C:15](=[O:19])[O:16][CH2:17][CH3:18])[CH2:12][CH2:13]1

Participants

4

Reactant 1

HCID 19761221HCID 19761221, compound

Product 1

HCID 19761240HCID 19761240, compoundYield 61%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 176Acetic AcidSolvent

Procedure

49 g of the compound obtained in Stage A dissolved in 500 ml of acetic acid in the presence of 1 g of 5% Pd/C are hydrogenated at 50° C. under 5 Kg. The catalyst is filtered off, the filtrate is evaporated, recovered with diethyl ether and rendered basic in the cold with 50 ml of sodium hydroxide solution. The ethereal phase is dried and evaporated to yield the desired compound.

Workup

  1. customare hydrogenated at 50° C. under 5 Kg
  2. filtrationThe catalyst is filtered off
  3. customthe filtrate is evaporated
  4. customrecovered with diethyl ether
  5. customThe ethereal phase is dried
  6. customevaporated

Sources & evidence

ORD record
ord-8f713f221d2b434b9db3a118adc7e30b
Source dataset
uspto-grants-1993_02
Patent number
US05189045

Reaction notes

Loading…