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Water → 2-Methyl-6-[3-(5-methyl-2-m-tolyloxazol-4-ylmethoxy)propoxymethyl]benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Iodomethyl-5-methyl-2-m-tolyloxazole | HCID 21980308 | — |
| 反応物 | Tert-butyl 2-(3-hydroxypropoxymethyl)-6-methylbenzoate | HCID 59341259 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 2-Methyl-6-[3-(5-methyl-2-m-tolyloxazol-4-ylmethoxy)propoxymethyl]benzoic acid | HCID 11990723 | — |
反応手順
200 mg of tert-butyl 2-(3-hydroxypropoxymethyl)-6-methylbenzoate are dissolved in 1.0 ml of MTBE, and 57 mg of sodium hydride (60% in mineral oil) are added. After gas evolution ceases, 446 mg of 5-methyl-2-m-tolyloxazol-4-ylmethyl iodide are added, and the suspension is stirred at RT overnight. Water is then added, and the solution is poured into a kieselguhr cartridge (VARIAN CHEM ELUT 1010). The product is eluted with MTBE and concentrated. The residue is dissolved without purification in DCM/TFA (3:1) and stirred at 40° C. for 5 h. The solution is concentrated and purified by prep. HPLC, resulting in 202 mg of 2-methyl-6-[3-(5-methyl-2-m-tolyloxazol-4-ylmethoxy)propoxymethyl]benzoic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07732471B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-263c2656eec34944ab4338ccd0d445ca |
| 出典メモ | uspto-grants-2010_06 |