Reference of 945950-37-8, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 945950-37-8, name is 4-Methyl-7H-pyrrolo[2,3-d]pyrimidine. A new synthetic method of this compound is introduced below.
a- Synhtesis of Int. 402: A sol. of 4-methyl-7H-pyrrazolo[2,3-d]pyrimidine (3.11 g, 23.4 mmol) in DMF (40 mL) was cooled to 0C and treated with NaH 60% (1.40 g, 35.0 mmol). The r.m. was stirred at 0C for 2h then 2-(trimethylsilyl)ethoxymethyl chloride (4.96 mL, 28.0 mmol) was added. The r.m. was stirred at r.t. for 2h and diluted in EtOAc. The organic layer was washed with water and brine (twice), dried over MgS04 and evaporated in vacuo to give brown oil. The oil was purified by prep. LC (irregular SiOH 15-40 muiotaeta, 80g, Grace, mobile phase gradient: from DCM 100% to DCM 96%, MeOH 4%). The desired fractions were collected and solvent evaporated until dryness to give 3.53 g. The residue was purified by prep. LC (irregular SiOH 15-40 muiotaeta, 80g, Grace, mobile phase gradient: from DCM 100% to DCM 96%, MeOH 4%). The pure fractions were collected and solvent evaporated until dryness to give 1.56 g of Int. 402 as a brown oil (25%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,945950-37-8, its application will become more common.
Reference:
Patent; JANSSEN PHARMACEUTICA NV; MEVELLEC, Laurence, Anne; PASQUIER, Elisabeth, Therese, Jeanne; DESCAMPS, Sophie; MERCEY, Guillaume, Jean, Maurice; WROBLOWSKI, Berthold; VIALARD, Jorge, Eduardo; MEERPOEL, Lieven; JEANTY, Matthieu, Ludovic; JOUSSEAUME, Thierry, Francois, Alain, Jean; WO2015/144799; (2015); A1;,
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