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Octylmethylamine → 2-[(4-Methoxy-benzenesulfonyl)-methyl-amino]-3-methyl-5-[2-(methyl-octyl-carbamoyl)-vinyl]-benzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Octylmethylamine | HCID 75538 | — |
| 反応物 | 5-(2-Carboxy-vinyl)-2-[(4-methoxy-benzenesulfonyl)-methyl-amino]-3-methyl-benzoic acid methyl ester | HCID 70055195 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[(4-Methoxy-benzenesulfonyl)-methyl-amino]-3-methyl-5-[2-(methyl-octyl-carbamoyl)-vinyl]-benzoic acid methyl ester | HCID 70053755 | 84% |
反応手順
A mixture of 182.6 mg (0.43 mmol) of the product of Example 204, 183 mg of molecular sieves and 105.8 mg (0.65 mmol) of 1,1'-dicyclohexylcarbodiimidazole in 4 ml THF was stirred for 1 h under nitrogen. A solution of N-methyloctylamine in 0.5 ml THF was then added to the reaction and the mixture was stirred for 18 hr at room temperature. The resulting mixture was filtered and the filtrate was diluted with ethyl acetate, washed with water and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue was chromatographed on silica gel eluting with EtOAc/Hexane (1:1) to provide 200 mg (84%) of the desired product as a colorless oil. Electrospray Mass Spec 545(M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05929097 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-925866f7b42b4849b1ffa781ad5ca878 |
| 出典メモ | uspto-grants-1999_07 |