Lawesson's reagent → HCID 18992239, compound

HRID 375616Notes

Reaction equation

HRID 375616 reaction equation
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:27])=CC=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[S:27])[N:7]3[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:8]3=[N:9]2)=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 139119483-Methyl-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one

Product 1

HCID 18992239HCID 18992239, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

9 g of 3-methyl-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazolin-12-one was treated with 15 g of Lawesson's reagent in toluene at reflux under nitrogen until the starting material was consumed, checked by TLC, using chloroform as eluent (24 hours). The mixture was concentrated in vacuo and chromatographed on silica gel, using chloroform as eluent. The bright yellow material was recrystallized from hexane-ethyl acetate.

Workup

  1. temperatureat reflux under nitrogen until the starting material
  2. customwas consumed
  3. custom(24 hours)
  4. concentrationThe mixture was concentrated in vacuo
  5. customchromatographed on silica gel
  6. customThe bright yellow material was recrystallized from hexane-ethyl acetate

Sources & evidence

ORD record
ord-154dedbd85924c5c9e7fb377657d0cc0
Source dataset
uspto-grants-1996_01
Patent number
US05486512

Reaction notes

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