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Sodium Thiosulfate → HCID 53236719、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 反応物 | 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine | HCID 58541899 | — |
| 反応物 | 2-(2,4-Dimethyl-thiazol-5-yl)-5-methoxy-benzaldehyde | HCID 58542002 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 53236719 | HCID 53236719 | 43% |
反応手順
To a solution of 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (100 mg, 0.39 mmol) in DMF (5 mL) is added 2-(2,4-dimethyl-thiazol-5-yl)-5-methoxy-benzaldehyde (144 mg, 0.58 mmol) at room temperature. Oxone (239 mg, 0.39 mmol) in H2O (1 mL) is added and the solution is stirred for 4 hours. Saturated sodium thiosulfate solution (5 mL) is added and the mixture is extracted with EtOAc (3×10 mL) and H2O (10 mL). The combined organic layer is dried with MgSO4 and is filtered. The filtrate is concentrated and the residue is purified by silica gel flash column chromatography eluting with 10% MeOH in CH2Cl2 to afford the title compound (81 mg, 43%) as a pale brown foam. LCMS (ESMS): m/z 485.72 (M++1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08420655B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-cd15a7c7d9474ab8961fb4ebf8bd6bbd |
| 出典メモ | uspto-grants-2013_04 |