化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 6-Iodobenzo[d][1,3]dioxol-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-(6-Iodo-2H-1,3-benzodioxol-5-yl)acetamide | HCID 53488067 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Iodobenzo[d][1,3]dioxol-5-amine | HCID 53488068 | 98.5% |
反応手順
A solution of N-(6-iodobenzo[d][1,3]dioxol-5-yl)acetamide (200 mg, 0.656 mmol) and NaOH (1.31 g, 32.8 mmol) in ethanol (26 mL) and water (6 mL) was heated to reflux with stirring for 4 h. The mixture was cooled and the solvent was removed under vacuum. The residue was partitioned between methylene chloride (100 mL) and water (100 mL). The organic layer was washed with water (2×100 mL), dried (MgSO4) and evaporated under vacuum to give 6-iodobenzo[d][1,3]dioxol-5-amine (170 mg, 98%) as orange solid. LCMS: 264 [M+1]+; 1H NMR (DMSO-d6) δ 4.88 (s, 2H), 5.87 (s, 2H), 6.47 (s, 1H), 7.07 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722703B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-860f375ec3cd4d27b866690d10ed8b72 |
| 出典メモ | uspto-grants-2014_05 |