Methyl isothiocyanate → 2-Thiophenecarboxylic acid, 2-[(methylamino)thioxomethyl]hydrazide
Reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([NH:8][NH2:9])=[O:7].[CH3:10][N:11]=[C:12]=[S:13]>C1COCC1>[C:2]1([C:6]([NH:8][NH:9][C:12]([NH:11][CH3:10])=[S:13])=[O:7])[S:1][CH:5]=[CH:4][CH:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A stirred mixture of 2-thiophene carboxylic acid hydrazide (4.75 g, 3.34×10-2 mole) and THF (115 ml) was warmed with a heat gun until homogeneous. A solution of freshly distilled methyl isothiocyanate (2.56 g, 3.51×10-2 mole) and THF (5 ml) was then added dropwise. After being stirred for about 14 hours the precipitate was collected by filtration, washed with a little Et2O, and dried by suction affording a colorless powder: 7.1 g (99%).
Workup
- temperaturewas warmed with a heat gun until homogeneous
- filtrationwas collected by filtration
- washwashed with a little Et2O
- customdried by suction
- customaffording a colorless powder
Sources & evidence
- ORD record
- ord-d2c4f39958a845f0a1e0bac0f30af068
- Source dataset
- uspto-grants-1991_01
- Patent number
- US04981863
Reaction notes
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