Ammonium formate → N,N-dimethylmorpholine-2-carboxamide

A mixture of 4-benzyl-N,N-dimethylmorpholine-2-carboxamide (803 mg, 3.23 mmol), ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) in EtOH (20 mL) was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated, and the residue was dissolved in EtOH (20 mL). Ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) were added to the mixture. The mixture was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated to afford desired product (506 mg, 98.9%) as colorless oil.

1. temperatureAfter cooling to room temperature
2. filtrationthe catalyst was filtered off
3. washwashed with EtOH
4. concentrationThe combined filtrate and washings were concentrated
5. dissolutionthe residue was dissolved in EtOH (20 mL)
6. temperatureThe mixture was heated at 50° C. for 1 hour
7. temperatureAfter cooling to room temperature
8. filtrationthe catalyst was filtered off
9. washwashed with EtOH
10. concentrationThe combined filtrate and washings were concentrated

ORDレコード

ord-25c055a7a16c471fb048b310c0e74a8d

出典データセット

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08609688B2