참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzyl Alcohol | HCID 244 | — |
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 4-methoxy-2,5-dihydro-1H-pyrrol-2-one | HCID 574769 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Benzyloxy-3-pyrrolin-2-one | HCID 2724741 | — |
반응 단계
5.7 g (50 mmol) of 4-methoxy-3-pyrrolin-2-one and 10.8 g (100 mmol) of benzyl alcohol were mixed with 0.4 g (4 mmol) of methanesulfonic acid and stirred for 24 hours at 80° C. and 20 mbars. Then the reaction solution was mixed with 50 ml of ice water and 100 ml of methylene chloride, and neutralized with 4 ml of saturated NaHCO3 solution. The aqueous phase was extracted twice with 50 ml of methylene chloride each. After drying of the organic phase over Na2SO4 and distilling off of the solvent, the residue was mixed with 150 ml of ice water, heated to 100° C. and azeotropically distilled off with 100 ml of water-benzyl alcohol. The crystals precipitated during cooling were recrystallized hot from 50 ml of toluene. 6.7 g of white, crystalline product with a melting point of 147° to 148° C. was obtained:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04855451 |
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| 출처 데이터셋 | uspto-grants-1989_08 |
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| ORD ID | ord-04e440d11a534283a9a851cb36ad1d00 |
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| 출처 메모 | uspto-grants-1989_08 |
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