ChemicalBook CAS DataBase List methyl sulfamate

methyl sulfamate synthesis

6synthesis methods

Product Name:methyl sulfamate
CAS Number:55665-95-7
Molecular formula:CH5NO3S
Molecular Weight:111.12

67-56-1 Synthesis

67-56-1
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55665-95-7
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Yield:55665-95-7 79.6%

Reaction Conditions:

with pyridine;dmap;sulphamoyl chloride in chloroform at -5 - 0; for 0.166667 h;Inert atmosphere;Solvent;Reagent/catalyst;

Steps:

1.2; 2.2; 3.2; 4.2; 5.2; 6 2. Preparation of methyl sulfamate
57.8g (0.5mol) of aminosulfonyl chloride, 300ml of chloroform and 6.1g (50mmol) of 4-dimethylaminopyridine (DMAP) were added to a 500ml three-necked flask, protected with nitrogen, and the temperature was lowered to -5 to 0 °C with stirring.Controlled temperature below 0 ° C, 19.4 g (0.6 mol) of methanol and 0.705 mol of pyridine were added dropwise.Stir for 10 minutes after the addition. The solvent was evaporated under reduced pressure, and ethyl acetate and ethyl acetate (200 ml) was added, and the mixture was stirred for 5 minutes, and the mixture was allowed to stand, and the organic layer was washed with 100 ml of 0.1 N hydrochloric acid.Washed with 200 ml of water and 100 ml of saturated brine, dried over anhydrous sodium sulfate.A liquid product of 44.2 g was obtained, which was cured below 20 °C. The yield was 79.6% and the purity was 97.1%. It was confirmed by MS, 1H-NMR and 13C-NMR structure that it was consistent with the reference pattern.

References:

Chongqing Pharmaceutical College;Shao Qian;He Dongxian;Yang Zhiguo;Li Yan CN110240552, 2019, A Location in patent:Paragraph 0027; 0032-0035; 0040-0043; 0048-0051; 0056-0059

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67-56-1 Synthesis

67-56-1
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7778-42-9 Synthesis