関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Phenylpropyl isocyanate | HCID 3427666 | — |
| 反応物 | Ethyl 3-(3'-methylaminobiphenyl-4-yl)propanoate | HCID 67271940 | — |
| 溶媒 | Triethylamine methylene chloride | HCID 21882572 | — |
| 生成物 | Ethyl 3-{3'-[1-methyl-3-(3-phenylpropyl)ureido]biphenyl-4-yl}propanoate | HCID 67272529 | 96.6% |
反応手順
188 μL (1.2 mmol, 1.5 eq) 3-phenylpropyl isocyanate are added to a solution of 230 mg (0.81 mmol, 1 eq) of ethyl 3-(3′-methylaminobiphenyl-4-yl)propanoate (prepared in Example 7c) in 10 mL of an 8/2 dichloromethane/triethylamine mixture. The reaction medium is stirred at 40° C. for 12 hours and then hydrolyzed with water and extracted with ethyl acetate. The organic phases are combined, washed with sodium chloride solution and dried over sodium sulfate. The solvents are evaporated off and the residual oil is chromatographed on silica (7/3 heptane/ethyl acetate). 348 mg of ethyl 3-{3′-[1-methyl-3-(3-phenylpropyl)ureido]biphenyl-4-yl}propanoate are obtained in solid form. Yield=96%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07863332B2 |
|---|
| 出典データセット | uspto-grants-2011_01 |
|---|
| ORD ID | ord-a1543b0243a846b2837b49971130c72e |
|---|
| 出典メモ | uspto-grants-2011_01 |
|---|