HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18617848, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | MeOH tetrahydrofuran | HCID 21899815 | — |
| Reactant | HCID 54545751 | HCID 54545751 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18617848 | HCID 18617848 | 61.8% |
Reaction Steps
To a solution of 4-(7H-pyrrolo[2,3-d]pyrimidin-6-yl)-benzoic acid methyl ester (0.601 g, 2.4 mmol) (reference example 43a) in 1:1 THF-methanol (10 mL) is added NaOH (10N) (2.4 mL, 24 mmol) and 0.5 ml H2O. The resulting solution is stirred for 1 hour then cooled to 0°-5° C. and adjusted to pH 3 with 2N HCl. The precipitated solid is filtered off, washed with a small volume of water and dried under high vacuum to give 0.355 g of title compound as a yellow solid. 1H NMR (DMSO) δ 7.59 (s, 1H), 8.10 (d, J=8 Hz, 2H), 8.20 (d, J=8 Hz, 2H), 9.22 (s, 1H), 9.50 (bs, 1H), 14.10 (bs, 1H). MS (EI) m/z 239 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06541505B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-37086d032f5a44e99e53298215e11521 |
| Source note | uspto-grants-2003_04 |