Lawesson's reagent → HCID 57195235, compound

HRID 847337Notes

Reaction equation

HRID 847337 reaction equation
[Cl:1][C:2]1[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:3]=1[O:4][C:5]1[CH:17]=[CH:16][C:8]2[N:9]([CH3:15])[C:10](=O)[CH:11]([CH3:13])[O:12][C:7]=2[CH:6]=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:35]2)=CC=1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:3]=1[O:4][C:5]1[CH:17]=[CH:16][C:8]2[N:9]([CH3:15])[C:10](=[S:35])[CH:11]([CH3:13])[O:12][C:7]=2[CH:6]=1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 11726718HCID 11726718, compound

Product 1

HCID 57195235HCID 57195235, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

7-(2-Chloro-4-trifluoromethylphenoxy)-2,4-dimethyl-2H-1,4-benzoxazine-3 (4H)-one (2.5 g) prepared in Example 6 was dissolved in toluene (30 ml), and 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (1.9 g) was added thereto, and the resultant mixture was refluxed for 2 hr. The solvent was distilled off in vacuo, and the residue was purified by silica gel column chromatography (developing solvent: n-hexane/ethyl acetate=5/1) to prepare the title compound (2.9 g) as a colorless crystal.

Workup

  1. distillationThe solvent was distilled off in vacuo
  2. customthe residue was purified by silica gel column chromatography (developing solvent: n-hexane/ethyl acetate=5/1)
  3. customto prepare the title compound (2.9 g) as a colorless crystal

Sources & evidence

ORD record
ord-7f6cc20123cf4b7e9c8d6f2f5e68df97
Source dataset
uspto-grants-1992_08
Patent number
US05141551

Reaction notes

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