Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
beta-Bromostyrene → 1-Methyl-2-styryl-2-hydroxy-6-piperidone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | beta-Bromostyrene | HCID 7667 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 2,6-Piperidinedione, 1-methyl- | HCID 161476 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-Methyl-2-styryl-2-hydroxy-6-piperidone | HCID 53776161 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04038273 |
| 출처 데이터셋 | uspto-grants-1977_07 |
| ORD ID | ord-ecfd5e6d54e74309bff4d1113272e89d |
| 출처 메모 | uspto-grants-1977_07 |