Methyl Isocyanate → HCID 20525165, compound

HRID 1702766Notes

Reaction equation

HRID 1702766 reaction equation
[CH3:1][N:2]=[C:3]=[O:4].[Cl:5][C:6]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:7]=1[CH:13]([OH:20])[CH2:14][N:15]1[CH:19]=[N:18][CH:17]=[N:16]1>C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC.C(OCC)(=O)C>[Cl:5][C:6]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:7]=1[CH:13]([O:20][C:3](=[O:4])[NH:2][CH3:1])[CH2:14][N:15]1[CH:19]=[N:18][CH:17]=[N:16]1

Participants

5

Reactant 2

HCID 12228Methyl IsocyanateHCID 66285758905-18-3

Product 1

HCID 20525165HCID 20525165, compoundYield 97%

Reagents, catalysts & solvents 2

HCID 9809426Di-n-butyldilauryltinCatalystHCID 8857Ethyl AcetateSolvent

Procedure

5.7 g (0.1 mol) of methyl isocyanate and a few drops of dibutyl-tin dilaurate were added, while stirring, to 25.8 g (0.1 mol) of 1-(2,4-dichlorophenyl)-1-hydroxy-2-(1,2,4-triazol-1-yl)-ethane in 250 ml of ethyl acetate. The mixture was stirred overnight at 60°-65° C. It was then allowed to cool and the crystalline precipitate was filtered off and washed with ether. 30.4 g (97% of theory) of 1-(2,4-dichlorophenyl)-1-methylcarbamoyloxy-2-(1,2,4-triazol-1-yl)-ethane of melting point 204° C. were obtained.

Workup

  1. temperatureto cool
  2. filtrationthe crystalline precipitate was filtered off
  3. washwashed with ether

Sources & evidence

ORD record
ord-a8d4aaff2d4745278e3067fd82f84fd3
Source dataset
uspto-grants-1982_09
Patent number
US04349556

Reaction notes

Loading…