Trifluoroacetic acid → 1-(Propan-2-yl)pyrrolidin-3-amine

t-Butyl-1-isopropylpyrrolidin-3-ylcarbamate (0.90 g, 3.9 mmol) obtained in Preparation Example (2-vii-1) was dissolved in dichloromethane (10 ml) in a 50 ml vessel, and trifluoroacetic acid (1.45 ml, 1.95 mmol, 5 eq.) was slowly added dropwise thereto while stirring. The resulting mixture was reacted for 18 hrs. After the completion of reaction, the reaction mixture was distilled and concentrated under reduced pressure, and then subjected to azeotropic distillation with CHCl3 3 times. The resultant was basified with aqueous 2N potassium hydroxide solution (20 ml) and extracted with CHCl3 3 times. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, filtered and distilled under reduced pressure to obtain 433 mg of the title compound as yellow oil (yield 86%).

1. customThe resulting mixture was reacted for 18 hrs
2. customAfter the completion of reaction
3. distillationthe reaction mixture was distilled
4. concentrationconcentrated under reduced pressure
5. distillationsubjected to azeotropic distillation with CHCl3 3 times
6. extractionextracted with CHCl3 3 times
7. customThe organic layer was separated
8. washwashed with brine
9. dry with materialdried over anhydrous magnesium sulfate
10. filtrationfiltered
11. distillationdistilled under reduced pressure

ORDレコード

ord-9f94af2bc61c4845a919ec70a10d2c50

出典データセット

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08053435B2