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beta-Bromostyrene → 1-Methyl-2-styryl-2-hydroxy-6-piperidone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | beta-Bromostyrene | HCID 7667 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2,6-Piperidinedione, 1-methyl- | HCID 161476 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methyl-2-styryl-2-hydroxy-6-piperidone | HCID 53776161 | — |
反応手順
The Grignard reagent prepared in 300 ml of THF from 24 g (1.0 mole) of magnesium and 42 g (0.30 mole) of β-bromostyrene is decanted from excess metal and added dropwise under nitrogen to a solution of 27 g (0.21 moles) of N-methyl glutarimide at 3°- 5°. After 11/2 hrs. at room temperature, the mixture is treated with 250 ml of saturated NH4Cl solution with cooling. The separated aqueous layer is reextracted and the combined THF extracts washed with salt, dried over MgSO4 and freed of solvent. Product is extracted into hot ether and crystallized on cooling to yield white crystals, mp 108°- 112° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04038273 |
| 出典データセット | uspto-grants-1977_07 |
| ORD ID | ord-ecfd5e6d54e74309bff4d1113272e89d |
| 出典メモ | uspto-grants-1977_07 |