Lawesson's reagent → HCID 22003612, compound

HRID 324502Notes

Reaction equation

HRID 324502 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:17]([C:18]3[C:19](=O)[NH:20][C:21](=[O:25])[N:22]([CH3:24])[CH:23]=3)[C:10]3[N:11]=[C:12]([CH3:16])[N:13]([CH2:14][CH3:15])[C:9]=3[CH:8]=[CH:7][C:6]=2[CH:27]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:37])=CC=1>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:17]([C:18]3[C:19](=[S:37])[NH:20][C:21](=[O:25])[N:22]([CH3:24])[CH:23]=3)[C:10]3[N:11]=[C:12]([CH3:16])[N:13]([CH2:14][CH3:15])[C:9]=3[CH:8]=[CH:7][C:6]=2[CH:27]=1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 22003572HCID 22003572, compound

Product 1

HCID 22003612HCID 22003612, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A mixture of the product of step (i) (0.065 g) and Lawesson's reagent (0.343 g) in 1,4-dioxane (5 ml) was heated at reflux for 20 hours. The solvent was evaporated under reduced pressure and the residue partitioned between dichloromethane and water. Purification was by chromatography eluting with 0.2% 880 ammonia, 4% methanol in dichloromethane to give the title compound.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 20 hours
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue partitioned between dichloromethane and water
  5. customPurification
  6. washeluting with 0.2% 880 ammonia, 4% methanol in dichloromethane

Sources & evidence

ORD record
ord-6fb525a8155846548a6aeb36704871e5
Source dataset
uspto-grants-2001_04
Patent number
US06218376B1

Reaction notes

Loading…