Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | HCID 86719398 | HCID 86719398 | — |
| Lösungsmittel | Water 2-methoxyethanol | HCID 22504935 | — |
| Produkt | HCID 86719405 | HCID 86719405 | 100,5% |
Reaktionsschritte
A mixture of (R)-tert-butyl 3-(4-amino-6-cyano-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)pyrrolidine-1-carboxylate (101) (290 mg, 0.58 mmol) and NaOH (290 mg, 7 mmol) in 2-methoxyethanol/H2O (8 mL/2 mL) was sealed in a microwave tube. The reaction mixture was purged with N2 (3×) and heated at 125° C. in a microwave reactor for 45 min. After cooling down to r.t., the reaction was diluted with water, and the resulting solid was filtered, washed with water, dried under vacuum. (R)-tert-Butyl 3-(4-amino-6-carbamoyl-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)pyrrolidine-1-carboxylate (125) (300 mg, quant.) was obtained as a brown solid. LC-MS (ESI): m/z (M+1) 515.0.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09062058B2 |
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| Quelldatensatz | uspto-grants-2015_06 |
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| ORD ID | ord-e4656a26f0dc4c5787930722d66918a0 |
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| Quellennotiz | uspto-grants-2015_06 |
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