3-Fluoro-4-Thiomorpholinoaniline synthesis
- Product Name:3-Fluoro-4-Thiomorpholinoaniline
- CAS Number:237432-11-0
- Molecular formula:C10H13FN2S
- Molecular Weight:212.29
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Yield:237432-11-0 99%
Reaction Conditions:
with hydrogen;palladium 10% on activated carbon in ethyl acetate; under 3000.3 Torr; for 6 h;
Steps:
3.3-3-2
3-3-2: Preparation of (3-fluoro-4-thiomorpholino)aniline To 100 ml of ethyl acetate were sequentially added 4.45 g (18.4 mmol) of (3-fluoro-4-thiomorpholino)nitrobenzene synthesized in Preparation Example 3-3-1 and 450 mg (10 W %) of Pd/C, followed by reaction in a hydrogen reactor under hydrogen pressure of 4bar for 6 hours. After the reaction was complete, Pd/C was filtered through celite. The filtrate was distilled under reduced pressure and purified by recrystallization from ethyl acetate and n-hexane. The resulting solid was dried under vacuum at about 40° to afford 3.86 g (yield: 99%) of the desired compound. Mass (M+): 213.0 1H-NMR (DMSO-d6): 2.69(brm, 4H), 3.00(brm, 4H), 5.03(d, 2H), 6.30(d, 2H), 6.78(t, 1H).
References:
US2011/306606,2011,A1 Location in patent:Page/Page column 14
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