関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 2,4-Dichloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 14116871 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 2-Chloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 5706774 | — |
反応手順
2,4-dichloro-7H-pyrrolo[2,3-d]pyrimidine (500 mg, 2.66 mmol), palladium(II)acetate (70 mg, 0.31 mmol) and BINAP (240 mg, 0.39 mmol) are dissolved in 6 mL THF and stirred for 20 min at 20° C. Then TMEDA (300 μL; 2.0 mmol) is added, the mixture is stirred for 20 min and then sodium borohydride (189 mg; 5.11 mmol) dissolved in 10 mL diglyme is added. After 1 h at 20° C. the mixture is combined with 1 N HCl and the solvent is eliminated in vacuo. The residue is purified by column chromatography (method prep. HPLC2; 3% acetonitrile to 55% in 12 min) and 2-chloro-7H-pyrrolo[2,3-d]pyrimidine (HPLC-MS: tRet.=1.25 min; MS(M+H)+=154; method FEC3) is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08637549B2 |
|---|
| 出典データセット | uspto-grants-2014_01 |
|---|
| ORD ID | ord-e27ea18f7072408ca17a6871a18001da |
|---|
| 出典メモ | uspto-grants-2014_01 |
|---|
