(3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-difluorophenyl)cyclopropyl)aMino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyriMidin-3-yl)-2,2- synthesis
- Product Name:(3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-difluorophenyl)cyclopropyl)aMino)-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyriMidin-3-yl)-2,2-
- CAS Number:274693-49-1
- Molecular formula:C24H28F2N6O3S
- Molecular Weight:518.58
220347-05-7
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Yield:274693-49-1 412.3 g
Reaction Conditions:
with toluene-4-sulfonic acid in ethanol; for 12.5 h;Reflux;
Steps:
5 Example 5 Preparation of compound 9
Under the room temperature condition, to a 2L four-necked round bottom flask was added reaction solvent ethanol 1L and 385 g compound (8) (0.83 mol). Slowly add 2,2-diethoxypropane 132 g (1 mol) and p-toluenesulfonic acid 8 g. After stirring for half an hour, heat to reflux, TLC monitoring reaction. After reaction 12 hours, finish. Lower to room temperature, [...] and sodium carbonate aqueous solution 500 ml washing, separating, the aqueous phase is butyl acetate extraction (3 * 1 L), the combined organic phase, through the concentrated under reduced pressure to obtain compound (9) crude product, crude product by the ethanol/water recrystallize to get intermediate (9) 412.3 g.
References:
CN107141298,2017,A Location in patent:Paragraph 0029
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