Dimethyl Sulfate → HCID 178502517, compound

HRID 1733374Notes

Reaction equation

HRID 1733374 reaction equation
[NH:1]=[C:2]1[C:15]([NH:16][C:17]([NH:19][C:20]([O:22][CH3:23])=[O:21])=[S:18])=[CH:14][CH:13]=[C:4]([C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[O:6])[CH:3]1[CH2:24][C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1.[H-].[Ca+2].[H-].[CH3:36]OS(OC)(=O)=O>COCCOC>[NH:1]=[C:2]1[C:15]([NH:16][C:17](=[N:19][C:20]([O:22][CH3:23])=[O:21])[S:18][CH3:36])=[CH:14][CH:13]=[C:4]([C:5]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[O:6])[CH:3]1[CH2:24][C:25]1[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=1

Participants

5

Reactant 3

HCID 6497Dimethyl SulfateHCID 3033859Calcium hydrideHCID 131711988HCID 131711988, compound

Product 1

HCID 178502517HCID 178502517, compound

Reagents, catalysts & solvents 1

HCID 80711,2-DimethoxyethaneSolvent

Procedure

To a mixture of 3-imino-(4-methoxyphenyl)methyl-4-(3-carbomethoxythioureido)benzophenone (4.47 g.; 0.01 mol) in 1,2-dimethoxyethane (50 ml.) there is added calcium hydride (0.42 g.; 0.01 mol). The mixture is refluxed for one hour and is cooled to room temperature. To the mixture there is added dimethylsulfate (1.26 g.; 0.01 mol). The mixture is stirred at room temperature for one hour and is poured into an excess of ice water. The suspension formed is filtered and the filter cake dried to afford 3-imino-(4-methoxyphenyl)methyl-4-(3-carbomethoxy-S-methylisothioureido)benzophenone.

Workup

  1. temperatureThe mixture is refluxed for one hour
  2. customThe suspension formed
  3. filtrationis filtered
  4. customthe filter cake dried

Sources & evidence

ORD record
ord-c73edd5c2b6e41c3997ce14ad9e9c8df
Source dataset
uspto-grants-1980_12
Patent number
US04241079

Reaction notes

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