3-tert-butoxycarbonyl-7-chloro-6-dimethylaminocarbonylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine → 7-Chloro-6-[1-(6-methylpyridin-2-yl)-ethylthio]-2,3,4,5-tetrahydro-1h-benzo[d]azepine hydrochloride

関与物質

反応手順

Use a method similar to the Preparation 177, except that the alkylation is conducted at 0° C., to react 3-tert-butoxycarbonyl-7-chloro-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine with (R)-methanesulfonic acid 1-(6-methyl-pyridin-2-yl)-ethyl ester. Use a method similar to the General Procedure 1-5, basic workup, and a method similar to the General Procedure 2-2 to give the title compound as a white solid. MS (APCI+) m/z: 333 (M+H)+; ee >97%, tR=6.53 min. (Chiral HPLC: Chiralpak OJ 120 Å 4.6×250 mm, 45° C.; eluent: 20% isopropanol with 0.05% triethylamine in SFC, flow rate 2 mL/min, LTV detector at 234 nm).

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