Reaktion #58162

Reaktionsgleichung

piperidine-4-carboxylic acid [3-(4-fluoro-phenoxy)-phenyl]-amide hydrochloride

4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine

triethylamine

→

1-(5-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperidine-4-carboxylic acid [3-(4-fluoro-phenoxy)-phenyl]-amide

Ausbeute 69.0%

Lösungsmittel

iso-propanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas placed in a microwave vessel
2. 2
   SonstigeThe microwave vessel was sealed
3. 3
   EinengenThe mixture was concentrated
4. 4
   Sonstigeto remove most of the iso-propanol and triethylamine
5. 5
   WaschenThe residue was washed with methanol (2×15 mL)
6. 6
   Sonstigeto afford a brown solid
7. 7
   WaschenThe solid was washed with water (3×30 mL)
8. 8
   Sonstigedried overnight

Vorschrift

A mixture of piperidine-4-carboxylic acid [3-(4-fluoro-phenoxy)-phenyl]-amide hydrochloride (2.51 g, 7.16 mmol) and 4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine (1.00 g, 5.97 mmol) in iso-propanol (15 mL) was placed in a microwave vessel, followed by addition of triethylamine (2.5 mL, 18 mmol). The microwave vessel was sealed then heated in the microwave at normal absorbance at 190° C. for 60 min. The mixture was concentrated to remove most of the iso-propanol and triethylamine. The residue was washed with methanol (2×15 mL) to afford a brown solid. The solid was washed with water (3×30 mL) and dried overnight to afford 1-(5-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-piperidine-4-carboxylic acid [3-(4-fluoro-phenoxy)-phenyl]-amide (1.83 g, 69%) as a light-brown solid ((M+H)+: 446.3).

Quelle