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Dimethylformamide → 4Iodo-benzoic acid N'-(2,2-dimethyl-propionyl)-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Iodobenzoic acid | HCID 12085 | — |
| 反応物 | tert-Butyl carbazate | HCID 70091 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 生成物 | 4Iodo-benzoic acid N'-(2,2-dimethyl-propionyl)-hydrazide | HCID 69315906 | — |
反応手順
4-Iodobenzoic acid (5 g, 20.2 mmol) was dissolved in dimethylformamide (50 ml). To this was added tert-butyl carbazate (2.66 g, 20.2 mmol), HATU (9.2 g, 24.2 mmol), 1-hydroxybenzotriazole (2.7 g, 20.2 mmol) and N,N-diisopropylethylamine (10.5 ml, 60.5 mmol). The mixture was stirred for 17 hours at room temperature. The solvent was removed in vacuo and the residue partitioned between dichloromethane (75 ml) and saturated aqueous sodium bicarbonate solution (75 ml). The organic layer was washed with water (100 ml), brine (100 ml), dried over magnesium sulfate, filtered and the solvent removed in vacuo. The desired product was obtained as a cream solid (4.6 g, 12.7 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425555B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-42cdd1f4f85041759000fb71106a03b8 |
| 出典メモ | uspto-grants-2008_09 |