Methane → HCID 23053764, compound

HRID 1650151Notes

Reaction equation

HRID 1650151 reaction equation
C([N:8]1[CH2:13][CH2:12][N:11](CC2C=CC=CC=2)[CH2:10][CH:9]1[C:21]([O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[O:22])C1C=CC=CC=1.C>C(O)C.[Pd]>[CH2:24]([O:23][C:21]([CH:9]1[CH2:10][NH:11][CH2:12][CH2:13][NH:8]1)=[O:22])[CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]

Participants

5

Reactant 2

HCID 297MethaneHCID 23053765HCID 23053765, compound

Product 1

HCID 23053764HCID 23053764, compoundYield 92%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Conditions

Temperature
40 °C

Procedure

A solution of 25 g (63.5 mmoles) of the compound prepared in step A and 200 mg Pd(10%)/charcoal in 200 ml of ethanol was treated by H2 under pressure of 2.8 bars under stirring at 40° C. overnight. After filtration, the ethanol was evaporated off under reduced pressure and the crude residue, purified on a silica gel column using MeOH/CHCl3 (5:95, in vol.) as eluent, yielded 12.5 g (92%) of the title compound as a highly hygroscopic compound.

Workup

  1. filtrationAfter filtration
  2. customthe ethanol was evaporated off under reduced pressure
  3. customthe crude residue, purified on a silica gel column

Sources & evidence

ORD record
ord-79cf640999a345b19f37cb807af8e0c8
Source dataset
uspto-grants-1990_05
Patent number
US04923870

Reaction notes

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