Methyl triflate → 4-[4-(Piperidine-1-sulfonyl)-4,7-diaza-spiro[2.5]oct-7-yl]-7H-pyrrolo[2,3-d]pyrimidine

A solution of 1-(imidazole-1-sulfonyl)-piperidine (intermediate 13) (0.047 mmol) in dry CH2Cl2 (1 mL) was cooled to 0° C. and added trifluoro-methanesulfonic acid methyl ester (0.047 mmol). The reaction mixture was allowed to warm up freely to rt over a period of 4 h and then concentrated in vacuo. The residual oil was redissolved in dry CH3CN (1.5 mL), added a solution of 4-(4,7-diaza-spiro[2.5]oct-7-yl)-7H-pyrrolo[2,3-d]pyrimidine (intermediate 21) (0.047 mmol) in DMSO (1 mL) and then stirred at 50° C. for 3 h. The pure compound was obtained by standard preparative HPLC purification of the reaction mixture.

1. concentrationconcentrated in vacuo
2. dissolutionThe residual oil was redissolved in dry CH3CN (1.5 mL)
3. customThe pure compound was obtained by standard preparative HPLC purification of the reaction mixture

ORDレコード

ord-4b3909a539534107bae9adc235d5aba5

出典データセット

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09233964B2