関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | (3-Iodo-pyrazolo[3,4-b]pyridin-1-yl)-acetic acid tert-butyl ester | HCID 57978086 | — |
| 触媒 | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (3-Cyano-pyrazolo[3,4-b]pyridin-1-yl)-acetic acid tert-butyl ester | HCID 57978082 | — |
反応手順
A 250 mL flask was charged with (3-iodo-pyrazolo[3,4-b]pyridin-1-yl)-acetic acid tert-butyl ester (15.0 g), PdCl2(dppf) (3.0 g), Zn(CN)2 (4.96 g), DMF (200 mL) and H2O (14 mL). The flask containing the resultant suspension was degassed and backfilled with nitrogen gas repeatedly for 5 minutes, followed by addition of Pd2(dba)3 (3.85 g) to the reaction mixture. The reaction mixture was heated under N2 at 90° C. for 16 h, cooled to room temperature, diluted with H2O (800 mL) and filtered. The collected solid was washed with toluene (10 mL) to provide (3-cyano-pyrazolo[3,4-b]pyridin-1-yl)-acetic acid tert-butyl ester as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07777035B2 |
|---|
| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-2f25144b922d45e2bf3d664f480569b8 |
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| 出典メモ | uspto-grants-2010_08 |
|---|
