HCID 22714706, compound → HCID 22714710, compound

HRID 1281173Notes

Reaction equation

HRID 1281173 reaction equation
[OH:1][C:2]1([C:8]2([C:23]#[N:24])[C:18]3[CH:17]=[C:16]4[C:12]([CH2:13][CH2:14][N:15]4[S:19]([CH3:22])(=[O:21])=[O:20])=[CH:11][C:10]=3[CH2:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1>[Ni].CO>[NH2:24][CH2:23][C:8]1([C:2]2([OH:1])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]2)[C:18]2[CH:17]=[C:16]3[C:12]([CH2:13][CH2:14][N:15]3[S:19]([CH3:22])(=[O:21])=[O:20])=[CH:11][C:10]=2[CH2:9]1

Participants

4

Reactant 1

HCID 22714706HCID 22714706, compound

Product 1

HCID 22714710HCID 22714710, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 887MethanolSolvent

Procedure

5.5 g of the product obtained in Step 2 are dissolved in 250 ml of a 3.6N solution of ammoniacal methanol containing 2 mg of Raney nickel. The reaction mixture is hydrogenated for 24 hours at 60° C. under a pressure of 30 bar. After filtration and removal of the solvent by evaporation, the residue is taken up in dichloromethane, washed with water until neutral, dried and concentrated to isolate the expected product.

Workup

  1. filtrationAfter filtration and removal of the solvent
  2. customby evaporation
  3. washwashed with water until neutral,
  4. customdried
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-3068acfd313643bbb354820545cb54ad
Source dataset
uspto-grants-2002_09
Patent number
US06452015B2

Reaction notes

Loading…