4-Methylthiomorpholine synthesis
- Product Name:4-Methylthiomorpholine
- CAS Number:55675-72-4
- Molecular formula:C5H11NS
- Molecular Weight:117.21
Yield:55675-72-4 78%
Reaction Conditions:
Stage #1: Thiomorpholinwith sodium hydride in tetrahydrofuran at 0; for 0.5 h;
Stage #2: methyl iodide in tetrahydrofuran at 0 - 20; for 1 h;
Steps:
[0045] Piocedui e for prepaialion of 1 -Methyl thiomorpholine. Thiomorphoiiuo ( 1.0 g, 9.7 mmol) was added to a stirred solution of NaI 1 (0.27 g. 1 1.6 mmol) in dry FHF (2>1 riL), ander argon at 00C. After 30 min methyliodide (2.0 g, 14.5 mmol) was added and stirred the reaction mixture for 1 h. ar room temperature. Then the reaction mixture was cooled to 0 C and quenched w ith small portion of ice and extracted with ethylacelate. Organic layer was washed with saturated NaCl solution and dried over NaSOa. evaporated under reduced pressure purified by column chromatography on neutral alυraina, eluting with CHCl3-MeOH (95:5), to give the 1- m ethyl thiomorpholine (78 %).
References:
WO2008/83038,2008,A1 Location in patent:Page/Page column 25
38280-81-8
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