Phosphorus sulfide (P2S5) → HCID 117974883, compound

HRID 2206854Notes

Reaction equation

HRID 2206854 reaction equation
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].[F:15][CH:16]([F:41])[C:17]1[C:21]([C:22]([NH:24][C:25]2[C:33]3[CH:32]([CH2:34][CH3:35])[O:31][C:30]([CH2:38][CH3:39])([CH2:36][CH3:37])[C:29]=3[CH:28]=[CH:27][CH:26]=2)=O)=[CH:20][N:19]([CH3:40])[N:18]=1>O1CCOCC1>[F:15][CH:16]([F:41])[C:17]1[C:21]([C:22](=[S:2])[NH:24][C:25]2[C:33]3[CH:32]([CH2:34][CH3:35])[O:31][C:30]([CH2:38][CH3:39])([CH2:36][CH3:37])[C:29]=3[CH:28]=[CH:27][CH:26]=2)=[CH:20][N:19]([CH3:40])[N:18]=1

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 71819569HCID 71819569, compound

Product 1

HCID 117974883HCID 117974883, compoundYield 61%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

In a microwave sealable tube, P2S5 (13 mg, 0.061 mmol, 0.5 eq) is added to a solution of 3-(difluoromethyl)-1-methyl-N-(1,1,3-triethyl-1,3-dihydro-2-benzofuran-4-yl)-1H-pyrazole-4-carboxamide (45 mg, 0.121 mmol, 1 eq) in 2 ml of dioxane. The tube is sealed and the reaction is microwaved 20 min at 130° C. The resulting solution is filtered through alumina and washed with dioxane. The solvent is evaporated and the residue purified by chromatography on silica gel to give pure material (61%)

Workup

  1. customThe tube is sealed
  2. customthe reaction is microwaved 20 min at 130° C
  3. filtrationThe resulting solution is filtered through alumina
  4. washwashed with dioxane
  5. customThe solvent is evaporated
  6. customthe residue purified by chromatography on silica gel

Sources & evidence

ORD record
ord-59c6df72ba1c482ba88efe022a469184
Source dataset
uspto-grants-2016_06
Patent number
US09375006B2

Reaction notes

Loading…