Acetic Acid → 2-(((1,1,1-Trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile

A solution of ethyl formate (330 mg, 4.46 mmol) and succinonitrile (300 mg, 3.75 mmol) in toluene (1561 μl) was added dropwise to a suspension of sodium methanolate (215 mg, 3.97 mmol) in toluene (1561 μl) at 0° C. After being stirred at RT for 3 h, the reaction mixture was treated with 1,1,1-trifluoro-2-methylpropan-2-amine (486 mg, 3.82 mmol) and acetic acid (255 μl, 4.46 mmol) then heated at 120° C. for 3 h. After being cooled to RT, the reaction mixture was washed with brine, then dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford the title compound as a brown oil, which was used without further purification.

1. temperaturethen heated at 120° C. for 3 h
2. temperatureAfter being cooled to RT
3. washthe reaction mixture was washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure

ORDレコード

ord-6830fa9bd52c4e4f868e2f2c20af2d0b

出典データセット

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09303045B2