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Water → 2-Chloro-4-isopropoxy-5-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Propanol, sodium salt (1:1) | HCID 10920443 | — |
| 反応物 | 2,4-Dichloro-5-nitropyridine | HCID 12275765 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-4-isopropoxy-5-nitropyridine | HCID 86697992 | 61% |
反応手順
3.38 g of sodium isopropoxide are added to a solution of 2.6 g of 2.4-dichloro-5-nitropyridine in 39 ml of DMF. The reaction medium is stirred at ambient temperature for 1 h 15 and 3.18 g of sodium isopropoxide are added. The reaction medium is stirred for a further 15 minutes and then the mixture is poured into 200 ml of water and extracted with ethyl acetate. The organic phase is dried over magnesium sulfate, filtered and concentrated under reduced pressure. Purification is carried out by flash chromatography on silica gel (40-63 microns), elution being carried out with a heptane/ethyl acetate mixture (90/10 to 80/20). 1.78 g of 2-chloro-5-nitro-4-(propan-2-yloxy)pyridine are obtained in the form of a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115140B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-6ce76442920749218b7376c694ac50e3 |
| 出典メモ | uspto-grants-2015_08 |