Aluminium lithium hydride → 2,2-Bis-(2,2,2-trifluoro-ethyl)-propane-1,3-diamine

340 mg LiAlH4 (8.95 mmol) was suspended in 15 ml dry Et2O and cooled in an ice bath. A solution of 760 mg 2,2-Bis-(2,2,2-trifluoro-ethyl)-malononitrile in Et2O was added dropwise at such a rate that the temperature was kept below 20° C. The mixture was stirred overnight at room temperature, cooled in an ice bath, and quenched by adding H2O (0.35 ml), 2M aqueous NaOH (0.70 ml), and again H2O (0.35 ml). The suspension was filtered, the filtercake was washed with Et2O, and the combined filtrates were evaporated to dryness under reduced pressure to give 0.72 g of an oil. This material was used in the subsequent step without further purification.

1. temperaturecooled in an ice bath
2. customwas kept below 20° C
3. temperaturecooled in an ice bath
4. customquenched
5. additionby adding H2O (0.35 ml), 2M aqueous NaOH (0.70 ml), and again H2O (0.35 ml)
6. filtrationThe suspension was filtered
7. washthe filtercake was washed with Et2O
8. customthe combined filtrates were evaporated to dryness under reduced pressure

ORDレコード

ord-64914aac893b45258fadccef246221ed

出典データセット

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08722887B2