Methylamine → {[3,5-Bis(trifluoromethyl)phenyl]methyl}(methyl)amine

温度

50 °C

Methylamine (3 g, 40% aqueous solution) was dissolved in 30 mL of MeOH. The reaction mixture was heated at 50° C. under stirring. 3,5-Bis(trifluoromethyl)-benzyl chloride (2 g, 7.6 mmol) dissolved in 10 mL of MeOH, was added. The solution was left stirring at this temperature for 5 h. The solution was concentrated carefully to remove MeOH as much as possible, then an aqueous solution of NaOH 1M was added and the aqueous layer was extracted with DCM. The two phases were separated; the organic phase was filtered through a phase separator and removed carefully in vacuo obtaining the title compound (0.8 g) as a yellow oil. UPLC-MS: m/z (ES+): 258.01 [M+H]+ Rt=0.60. 1H NMR (400 MHz, CDCl3) δ ppm 7.83 (s, 2H), 7.79 (s, 1H), 3.91 (s, 2H), 3.30 (m, 1H), 2.50 (s, 3H); UPLC-MS: Rt=1.30; m/z (ES+): 586 [M+H]+.

1. additionwas added
2. waitThe solution was left
3. stirringstirring at this temperature for 5 h
4. concentrationThe solution was concentrated carefully
5. customto remove MeOH as much as possible, then an aqueous solution of NaOH 1M
6. additionwas added
7. extractionthe aqueous layer was extracted with DCM
8. customThe two phases were separated
9. filtrationthe organic phase was filtered through a phase separator
10. customremoved carefully in vacuo

ORDレコード

ord-08bf3a079d804209965d1770ab8d4eb3

出典データセット

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09181259B2