反应 #3000978
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08063099B2
反应条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 5-Bromo-2-chloro-pyrimidine (18.4 mmol) is added to a solution of (1S,2S,5R)-2-aminomethyl-3-aza-bicyclo[3.1.0]hexane-3-carboxylic acid tert-butyl ester (14.1 mmol) in o-xylene (30 mL). K2CO3 (42.4 mmol) and DIPEA (42.4 mmol) are added successively and the mixture is heated to 140° C. for 17 h. The mixture is cooled to RT and diluted with EtOAc (100 mL) and water (100 mL). The layers are separated and the aq. layer is extracted with DCM (100 mL). The combined organic layers are dried over MgSO4 and concentrated in vacuo. The obtained brownish solid is stirred in ether (75 mL). The suspension is filtered and washed with ether (25 mL) and the residue is dried in vacuo to give the desired product. The mixture is cooled to RT The layers are separated the aq. layer is extracted with DCM (100 mL) The combined organic layers are dried over MgSO4 concentrated in vacuo The suspension is filtered washed with ether (25 mL) the residue is dried in vacuo
来源 ID: ord-4ef632e3b9b7411e90c7c9c26ee59a42