Lawesson's reagent → HCID 22003601, compound

HRID 324503Notes

Reaction equation

HRID 324503 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:18]([C:19]3[C:20](=O)[NH:21][C:22](=[O:26])[N:23]([CH3:25])[CH:24]=3)[C:10]3[N:11]=[C:12]([CH3:17])[N:13]([CH:14]4[CH2:16][CH2:15]4)[C:9]=3[CH:8]=[CH:7][C:6]=2[CH:28]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:38])=CC=1>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:18]([C:19]3[C:20](=[S:38])[NH:21][C:22](=[O:26])[N:23]([CH3:25])[CH:24]=3)[C:10]3[N:11]=[C:12]([CH3:17])[N:13]([CH:14]4[CH2:16][CH2:15]4)[C:9]=3[CH:8]=[CH:7][C:6]=2[CH:28]=1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 22003658HCID 22003658, compound

Product 1

HCID 22003601HCID 22003601, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A mixture of the product of step (i) (0.070 g) and Lawesson's reagent (0.350 g) in 1,4-dioxane (5 ml) was heated at reflux for 8 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, 2% methanol in dichloromethane to give the title compound.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 8 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, 2% methanol in dichloromethane

Sources & evidence

ORD record
ord-223c9fd59dc841fd96597b5a45a92a7c
Source dataset
uspto-grants-2001_04
Patent number
US06218376B1

Reaction notes

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