Triethylamine → HCID 18944991, compound

HRID 399735Notes

Reaction equation

HRID 399735 reaction equation
[CH3:1][C:2]([CH3:37])([P:34](=[O:36])=[O:35])[N:3]([C:13]1[CH:18]=[C:17]([O:19][CH2:20][CH2:21][NH:22][C:23]2[C:28](Cl)=[C:27](Cl)[N:26]=[C:25](Cl)[C:24]=2Cl)[CH:16]=[C:15]([CH3:33])[CH:14]=1)[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5].C(N(CC)CC)C>CO.[Pd]>[CH3:1][C:2]([CH3:37])([P:34](=[O:36])=[O:35])[N:3]([C:13]1[CH:18]=[C:17]([O:19][CH2:20][CH2:21][NH:22][C:23]2[CH:28]=[CH:27][N:26]=[CH:25][CH:24]=2)[CH:16]=[C:15]([CH3:33])[CH:14]=1)[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5]

Participants

5

Reactant 2

HCID 8471TriethylamineHCID 86753227HCID 86753227, compound

Product 1

HCID 18944991HCID 18944991, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

0.2 g (0.33 mmol) N-(dimethyloxophosphinyl-methyl)-N-{3-methyl-5-[2-(2,3,5,6-tetrachloropyridin-4-ylamino)-ethoxy]-phenyl}-benzenesulfonamide in 10 ml methanol was hydrogenated in the presence of 0.28 ml triethylamine and 0.1 g 10% palladium on carbon at room temperature and normal pressure. After 18 hours it was filtered, the residue was dissolved in 3 ml ethanol, 30 ml ether was added, it was filtered, washed with ether and 0.12 g (77%) of the title compound of Fp. 228°-232° C. was obtained.

Workup

  1. filtrationAfter 18 hours it was filtered
  2. dissolutionthe residue was dissolved in 3 ml ethanol
  3. addition30 ml ether was added
  4. filtrationit was filtered
  5. washwashed with ether and 0.12 g (77%) of the title compound of Fp
  6. custom228°-232° C. was obtained

Sources & evidence

ORD record
ord-dd57939c0830468f955a173788facb91
Source dataset
uspto-grants-1998_10
Patent number
US05824679

Reaction notes

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