2-tert-Butyl-1,1,3,3-tetramethylguanidine → 4-(3,3-Difluoro-cyclobutylamino)-5-methanesulfonyl-2-methyl-benzoic acid methyl ester

温度

150 °C

0.70 g of N-(3,3-Difluoro-cyclobutyl)-methanesulfonamide, 0.93 g of 4-fluoro-5-methanesulfonyl-2-methyl-benzoic acid methyl ester, and 1.5 ml of N″-tert-butyl-N,N,N′,N′-tetramethyl-guanidine were dissolved using 10 ml NMP (anhydrous) and stirred for 6 h at 150° C. The reaction mixture was cooled to ambient temperature and 200 ml of EE added. This solution was washed three times using 20 ml of a saturated aqueous NaHSO4-solution each time. Thereafter, the organic layer was washed three times using 30 ml of a saturated aqueous Na2CO3-solution each time. The organic layer was dried over MgSO4 and the solvent removed in vacuo. Chromatography on silica gel using DIP yielded 220 mg of a colourless foam.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. addition200 ml of EE added
3. washThis solution was washed three times
4. washThereafter, the organic layer was washed three times
5. dry with materialThe organic layer was dried over MgSO4
6. customthe solvent removed in vacuo

ORDレコード

ord-6fd7de97231d49aaadb4d63c23af7c18

出典データセット

uspto-grants-2005_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06878748B2