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Iodoethane → 6-(6-chloro-pyrimidine-4-carbonyl)-3-ethyl-4-methyl-3H-benzoxazol-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one | HCID 58181206 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(6-chloro-pyrimidine-4-carbonyl)-3-ethyl-4-methyl-3H-benzoxazol-2-one | HCID 58181195 | — |
反応手順
44 mg (1.0 mmol) sodium hydride (55%, suspension in mineral oil) were added to 0.25 g (0.86 mmol) 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one in 2.0 mL DMF and the mixture was stirred for 30 min at RT. Then 98 μL (1.2 mmol) ethyl iodide were added and the mixture was stirred for 1 h at RT. The reaction mixture was diluted with ice water and extracted with EtOAc. The organic phase was washed with water, dried on sodium sulphate, filtered and evaporated down i. vac. The residue was purified by flash chromatography. The fractions containing the product were combined and evaporated down.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08629137B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-bdfc72f949b04459a75172a578251f92 |
| 出典メモ | uspto-grants-2014_01 |