Hydrochloric Acid → HCID 20277898, compound

Temperature

0 °C

The N-benzyl-4-methyl-4-nitropentanoic acid amide (2.5 g) obtained above was dissolved in tetrahydrofuran (20 ml) and cooled to 0° C. 1 N Borane tetrahydrofuran complex (13 ml) was added dropwise thereto and then stirred overnight at room temperature. The reaction mixture was cooled again to 0° C., and 2 N hydrochloric acid (30 ml) was added thereto, followed by heating to 50° C. The reaction solution was extracted with ethyl acetate. The aqueous phase was alkalinized by 50% sodium hydroxide solution, extracted with chloroform. The extract was washed with a saturated saline solution, and dried over sodium sulfate anhydrous. The product was concentrated under reduced pressure to give benzyl-4-methyl-4-nitropentylamine (1.7 g, Y.: 73%) as a colorless oil.

1. addition1 N Borane tetrahydrofuran complex (13 ml) was added dropwise
2. temperatureThe reaction mixture was cooled again to 0° C.
3. temperatureby heating to 50° C
4. extractionThe reaction solution was extracted with ethyl acetate
5. extractionextracted with chloroform
6. washThe extract was washed with a saturated saline solution
7. dry with materialdried over sodium sulfate anhydrous
8. concentrationThe product was concentrated under reduced pressure

ORD record

ord-fb72614fa60049dd8777f0fcdaff8495

Source dataset

uspto-grants-2008_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07345180B2