Allylamine → HCID 65380380, compound

Allylamine (9.8 mL) was added to a solution of 1,2,3-trifluoro-5-((E)-2-nitrovinyl)benzene (6.6 g) in THF (30 mL). The reaction solution was stirred at room temperature for 2.5 hours and then concentrated under reduced pressure. Zinc powder (10.6 g) was added to a solution of the residue in ethanol (35 mL) and concentrated hydrochloric acid (35 mL) at 0° C., and the reaction solution was stirred at 0° C. for 30 minutes and at room temperature for 15 hours. The reaction solution was added to ice-cold aqueous ammonia, and the reaction mixture was subjected to extraction with chloroform. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 7.52 g of a crude product of the title compound. The property values of the compound are as follows.

1. concentrationconcentrated under reduced pressure
2. additionZinc powder (10.6 g) was added to a solution of the residue in ethanol (35 mL)
3. stirringconcentrated hydrochloric acid (35 mL) at 0° C., and the reaction solution was stirred at 0° C. for 30 minutes and at room temperature for 15 hours
4. additionThe reaction solution was added to ice-cold aqueous ammonia
5. extractionthe reaction mixture was subjected to extraction with chloroform
6. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure

ORD record

ord-f637c1287e7e4ef7b8871c6d674a8475

Source dataset

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08048878B2