Lawesson's reagent → HCID 19913710, compound

HRID 477797

Reaction equation

HRID 477797 reaction equation
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[N:9][NH:10][C:11]2=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:24])=CC=1>C(#N)C>[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH:8]=[N:9][NH:10][C:11]2=[S:24])=[CH:6][CH:5]=1)([O-:3])=[O:2]

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 2777297-Nitrophthalazin-1(2h)-one

Product 1

HCID 19913710HCID 19913710, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

13.9 g of 7-nitro-1(2H)-phthalazinone and 16.3 g of Lawesson reagent in 170 ml of acetonitrile are heated under reflux for 45 minutes. The reaction mixture is filtered while hot. The filtrate is cooled in an ice-bath and the crystals obtained are removed by filtration under suction. After drying in vacuo and recrystallization there is obtained 7-nitro-1(2H)-phthalazinethione as yellow crystals of m.p. 233+-234° (methanol/acetonitrile).

Workup

  1. temperatureunder reflux for 45 minutes
  2. filtrationThe reaction mixture is filtered while hot
  3. temperatureThe filtrate is cooled in an ice-bath
  4. customthe crystals obtained
  5. customare removed by filtration under suction
  6. customAfter drying in vacuo
  7. customrecrystallization there

Sources & evidence

ORD record
ord-50d8a50fdbe1468396f82690e98f86ca
Source dataset
uspto-grants-1989_12
Patent number
US04889854

Linked notes

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