Methyl chloroformate → HCID 178502065, compound
Reaction equation
[NH2:1][C:2]1[NH:6][N:5]=[N:4][N:3]=1.C(N(CC)CC)C.Cl[C:15]([O:17][CH3:18])=[O:16]>C(#N)C>[CH3:18][O:17][C:15](=[O:16])[NH:1][C:2]1[NH:6][N:5]=[N:4][N:3]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 5-Amino tetrazole (10.00 g, 117.56 mmol)/Triethyl amine (16.48 ml, 118.739 mmol) in acetonitrile was added Methyl chloroformate (9.1375 ml, 118.739 mmol) at 0° C. The reaction mixture was slowly brought to room temperature and stirred for about 30 minutes. After about 30 minutes the reaction warmed and was refluxed for about 2 hrs. The reaction was then cooled to room temperature and the solvent was removed under reduced pressure, leaving a residue. The residue was washed with dilyte HCl to yield a white-colored solid. The solid was then dried at 105 C for about 6 hrs, resulting in a 92% yield.
Workup
- customwas slowly brought to room temperature
- temperatureAfter about 30 minutes the reaction warmed
- temperaturewas refluxed for about 2 hrs
- customthe solvent was removed under reduced pressure
- customleaving a residue
- washThe residue was washed with dilyte HCl
- customto yield a white-colored solid
- customThe solid was then dried at 105 C for about 6 hrs
- customresulting in a 92% yield
Sources & evidence
- ORD record
- ord-9157ee50fb0545caae8292a05d8ccdd4
- Source dataset
- uspto-grants-2011_03
- Patent number
- US07914632B2
Reaction notes
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