Ammonia → N-trimethylsilylurethane
Reaction equation
[CH3:1][Si:2]([CH3:9])([CH3:8])[NH:3][Si](C)(C)C.N[C:11]([O:13][CH2:14][CH3:15])=[O:12].N>S1(C2C(=CC=CC=2)C(=O)N1)(=O)=O.C1(C)C=CC=CC=1>[CH3:1][Si:2]([CH3:9])([CH3:8])[NH:3][C:11]([O:13][CH2:14][CH3:15])=[O:12]Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Procedure
15.6 ml of hexamethyldisilazane (0.075 mole) were added over 2 minutes to a refluxing mixture of 8.9 g (0.1 mole) of urethane, 183 mg (1 mmole) of saccharin and 10 ml of toluene and the theoretical amount of ammonia was evolved in 30 minutes. Refluxing was continued for 15 minutes and the solvent and excess hexamethyldisilazane were removed under reduced pressure. The residue was vacuum distilled to obtain 15.6 g (96.9%) of N-trimethylsilylurethane boiling at 73° C. at 12 mm Hg and nD 25=1.4268.
Workup
- temperatureRefluxing
- customthe solvent and excess hexamethyldisilazane were removed under reduced pressure
- distillationdistilled
Sources & evidence
- ORD record
- ord-dcdf5a86e6d246da8c89c3c05a6d955b
- Source dataset
- uspto-grants-1983_08
- Patent number
- US04400509
Reaction notes
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