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Dimethyl Phthalate → HCID 178509848、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Phthalate | HCID 8554 | — |
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | 1-Pivaloyloxymethyl-3-(4-cyanobenzyl)-4-(2-phthalimidoethyl) imidazolium bromide | HCID 86755883 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178509848 | HCID 178509848 | — |
反応手順
1-Pivaloyloxymethyl-3-(4-cyanobenzyl)-4-(2-phthalimidoethyl) imidazolium bromide (1.00 g, 1.81 mmol) was dissolved in ethanol (50 mL), treated with hydrazine (0.287 mL, 9.06 mmol), and heated at reflux for 16 h. Dimethyl phthalate (2.22 mL, 13.57 mmol) was added and reflux was continued for 6 h. The reaction mixture was cooled in an ice-H2O bath, the solid precipitate filtered off, the filtrate concentrated to dryness, and the residue chromatographed (SiO2, CH2Cl2 (NH4OH): 3-8% CH3OH) to give the title compound. 1H NMR (CD3OD) δ 7.76 (s, 1H), 7.74 (d, 2H, J=8 Hz), 7.27 (d, 2H, J=8 Hz), 6.88 (s, 1H), 5.35 (s, 2H), 2.76 (t, 2H, J=6 Hz), 2.60 (t, 2 H, J=6 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06127390 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-3bd4b4962be24736b720693d111001fd |
| 出典メモ | uspto-grants-2000_10 |