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Sodium Carbonate → 5-Amino-1-chloroisoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1-Chloro-5-nitroisoquinoline | HCID 459774 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-Amino-1-chloroisoquinoline | HCID 459771 | — |
反応手順
A mixture of 1-chloro-5-nitroisoquinoline (450 mg, 0.0022 mol), stannous chloride dihydrate (2.4 g, 0.011 mol), and EtOAc (50 mL) was stirred under reflux under an atmosphere of nitrogen for 3 h. After cooling, the mixture was poured into ice-water and basified to pH 10.0 with aq. Na2CO3. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated under vacuum. The residue was purified by column chromatography on silica gel to give the product as a light yellow solid. LC-MS: 3.17 min, 179.2 & 181.2 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07312233B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-b7471276dcf14b909b6e0a0b1793c111 |
| 出典メモ | uspto-grants-2007_12 |