참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 5-[3-(4-Isopropoxy-3-methoxyphenyl)propyl]-2,4-oxazolidinedione | HCID 69830628 | — |
| 촉매 | Titanium Tetrachloride | HCID 24193 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-[3-(4-Hydroxy-3-methoxyphenyl)propyl]-2,4-oxazolidinedione | HCID 69830471 | 76% |
반응 단계
A solution of titanium tetrachloride (TiCl4) (10.6 g) in dichloromethane (10 ml) was added dropwise, at 0° C., to a solution of 5-[3-(4-isopropoxy-3-methoxy-phenyl)propyl]-2,4-oxazolidinedione (4.3 g) in dichloromethane (130 ml). The mixture was stirred for one hour at 0° C., which was poured into 2N HCl, followed by stirring for 15 minutes at room temperature. The organic layer was separated, and the aqueous layer was subjected to extraction with chloroform. The organic layers were combined, washed successively with water, 2N HCl and water, which was dried (MgSO4), followed by concentration to yield 5-[3-(4-hydroxy-3-methoxyphenyl)propyl]-2,4-oxazolidinedione (2.8 g, 76%). Recrystallization of the product from ethanol-hexane gave colorless prisms, m.p.147-148° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05932601 |
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| 출처 데이터셋 | uspto-grants-1999_08 |
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| ORD ID | ord-716fb1edf1f743da838b0944759ef5cf |
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| 출처 메모 | uspto-grants-1999_08 |
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