Phosphorus sulfide (P2S5) → HCID 178510895, compound

HRID 2231642Notes

Reaction equation

HRID 2231642 reaction equation
O=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([CH2:12][C:13]#[N:14])=[N:4][NH:3]1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:16]>N1C=CC=CC=1>[SH:16][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([CH2:12][C:13]#[N:14])=[N:4][N:3]=1

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 2409074HCID 2409074, compound

Product 1

HCID 178510895HCID 178510895, compoundYield 105.6%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

3,4-dihydro-4-oxo-1-phthalazin-acetonitrile (126 g) is suspended in anhydrous pyridine (1300 ml) under anhydrous conditions. P2S5 (230 g) is added portionwise to this suspension at room temperature and with stirring, then the mixture is slowly heated to reflux temperature and kept at this temperature for about 2 h. Pyridine is then evaporated under reduced pressure and the residue is poured into water (3 l). The solid which separates is recovered by filtration, thoroughly wshed first with water and then with cold dilutes aqueous ammonia. The recovered solid is oven-dried, yielding 4-mercapto-phthalazin-acetonitrile (110 g).

Workup

  1. temperaturethe mixture is slowly heated
  2. temperatureto reflux temperature
  3. customPyridine is then evaporated under reduced pressure
  4. additionthe residue is poured into water (3 l)
  5. filtrationThe solid which separates is recovered by filtration, thoroughly wshed first with water
  6. customThe recovered solid is oven-dried

Sources & evidence

ORD record
ord-85757a12b5254f90af15722aa2b4b989
Source dataset
uspto-grants-1988_11
Patent number
US04783461

Reaction notes

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