反应详情

温度

5 °C

To 1.2 g (3.7 mmol) of methyl 1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylate were successively added 13.5 cm3 of tetrahydrofuran, 0.47 g (11.2 mmol) of lithium hydroxyde, monohydrate and 13.5 cm3 of distilled water. The reaction mixture was heated at reflux temperature for 4 hours and then concentrated to dryness in vacuo (2.7 kPa). The residue was dissolved into 72 cm3 of distilled water and the mixture was extracted with 35 cm3 of ethyl acetate. The aqueous phase was cooled to about 5° C. and 10 cm3 of 1N hydrochloric acid were added dropwise (pH ca. 3). The resulting precipitate was filtered, washed twice with 20 cm3 of distilled water and dried in vacuo at about 50° C. to yield 0.93 g of 1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylic acid as off-white crystals. mp>260° C.; IR spectrum (KBr): 3461; 3152; 2951; 2571; 1678; 1590; 1544; 1452; 1263; 1204; 916; 808; 774; 746; 681 and 607 cm−1.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux temperature for 4 hours
3. concentrationconcentrated to dryness in vacuo (2.7 kPa)
4. dissolutionThe residue was dissolved into 72 cm3 of distilled water
5. extractionthe mixture was extracted with 35 cm3 of ethyl acetate
6. addition10 cm3 of 1N hydrochloric acid were added dropwise (pH ca. 3)
7. filtrationThe resulting precipitate was filtered
8. washwashed twice with 20 cm3 of distilled water
9. customdried in vacuo at about 50° C.