Dichloromethane → HCID 20231876, compound
Reaction equation
[NH:1]([C:3]([O:5]C)=[O:4])[NH2:2].[CH3:7][N:8]=[C:9]=[S:10].[CH2:11](Cl)Cl>>[CH3:11][N:1]([C:3]([OH:5])=[O:4])[NH:2][C:9]([NH:8][CH3:7])=[S:10]Participants
4
Conditions
- Temperature
- 40 °C
Procedure
To a stirred mixture of 20 g (0.22, 0.2 mole) methyl hydrazinocarboxylate in 150 ml methylene chloride, 14.6 g (0.2 mole) methyl isothiocyanate in 50 ml methylene chloride was added dropwise. The reaction mixture was refluxed at about 40° C. for 0.5 hour, was allowed to stir overnight at ambient temperature, and was refluxed an additional 2 hours. The reaction mixture was cooled, vacuum filtered and the solids were dried to give 27.2 g of the above-identified product.
Workup
- additionwas added dropwise
- temperaturewas refluxed an additional 2 hours
- temperatureThe reaction mixture was cooled
- filtrationvacuum filtered
- customthe solids were dried
Sources & evidence
- ORD record
- ord-3f065072038a4c96a6627cd53c49aea8
- Source dataset
- uspto-grants-1986_10
- Patent number
- US04616004
Reaction notes
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