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Sodium Hydroxide → 2-chloro-6-(3,5,5-trimethylhexyloxy)pyridine N-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3,5,5-Trimethyl-1-hexanol | HCID 18938 | — |
| 反応物 | 2,6-Dichloropyridine N-Oxide | HCID 817673 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-chloro-6-(3,5,5-trimethylhexyloxy)pyridine N-oxide | HCID 53824839 | — |
反応手順
The 0.82 g (0.0050 moles) of 2,6-dichloropyridine N-oxide and 0.80 g (90%) (0.0050 moles) of 3,5,5-trimethyl-1-hexanol was reacted with 0.206 g (0.0050 moles) of ground sodium hydroxide in 8.2 ml of DMSO at 80° C. for 8.5 hours to give 2-chloro-6-(3,5,5trimethylhexyloxy)pyridine N-oxide. It was reacted with 0.600 g (0.015 moles) of ground sodium hydroxide at 80° C. for 4 hours to give 1-hydroxy-6-(3,5,5-trimethyl-hexyloxy) pyridine-2(1H)-one. After cooling, it was added 74 ml of water and was adjusted with 6N HCL to pH 3. The precipitate was filtered and washed with water to give 0.577 g (45%). It was recrystallized from ethyl acetate and hexanes: mp 130.5°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424435 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-bf365ee63a3141adbc949b17123d9b8b |
| 出典メモ | uspto-grants-1995_06 |