関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Trimethylsilyldiazomethane | HCID 167693 | — |
| 反応物 | 2-(2-Benzylidenehydrazino)benzoic acid | HCID 222687 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 2-[2-benzylidenehydrazino]benzoate | HCID 67063589 | 100% |
反応手順
2-(N′-Benzylidene-hydrazino)-benzoic acid (5.0 g, 20.81 mmol) in 1:1 tetrahydrofuran and methanol (50 mL) was reacted with a solution of trimethylsilyl diazomethane in hexanes (2.0M, 12 mL, 25.0 mmol) at 0° C. for 1 hour then stirred at 25° C. for 48 hours. The solvent was removed under vacuum to give the title compound as a solid (6.00 g, 100%). 1H NMR (300 MHz, DMSO-d6) δ ppm 3.87 (s, 3 H) 6.84 (td, J=7.54, 1.10 Hz, 1 H) 7.41 (m, 3 H) 7.54 (m, 1 H) 7.74 (m, 3 H) 7.86 (dd, J=8.09, 1.47 Hz, 1 H) 8.21 (s, 1 H) 11.02 (s, 1 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07902203B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-77a3df5ed4f24f969050a3b7d82fe064 |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|
