Phosphorus sulfide (P2S5) → HCID 136045551, compound

HRID 2072702Notes

Reaction equation

HRID 2072702 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[C:22]4[CH:31]=[CH:30][S:29][C:23]=4[NH:24][C:25](=O)[CH2:26][N:27]=3)=[CH:17][CH:16]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:33]>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[C:22]4[CH:31]=[CH:30][S:29][C:23]=4[NH:24][C:25](=[S:33])[CH2:26][N:27]=3)=[CH:17][CH:16]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10]

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 136116068HCID 136116068, compound

Product 1

HCID 136045551HCID 136045551, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
25 °C

Procedure

To a solution of 0.6 g (1.4 mmol) of the compound prepared in (e) above in 30 ml of dry pyridine was added 0.37 g (0.82 mmol) of phosphorus pentasulfide, and the resultant mixture was heated to 90° C. and maintained at this temperature for 30 minutes under a nitrogen atmosphere. After cooling the reaction mixture to 25° C., the solvent was evaporated and the resultant residue was diluted with methylene chloride. The organic phase was then washed successively with water and brine, dried over anhydrous magnesium sulfate and evaporated to yield a red foam.

Workup

  1. temperaturemaintained at this temperature for 30 minutes under a nitrogen atmosphere
  2. customthe solvent was evaporated
  3. additionthe resultant residue was diluted with methylene chloride
  4. washThe organic phase was then washed successively with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated
  7. customto yield a red foam

Sources & evidence

ORD record
ord-cdf4f6f339574c729fee191edbc3d220
Source dataset
uspto-grants-1990_04
Patent number
US04914096

Reaction notes

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