참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 2-[4-(2-Oxopropoxy)phenyl]ethanol | HCID 21832165 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | HCID 21832202 | HCID 21832202 | — |
반응 단계
1.96 g of acetic anhydride were added, whilst ice-cooling, to a mixture of 3.1 g of 2-[4-(2-oxopropoxy)phenyl]ethanol (prepared as described in Preparation 7), 50 ml of anhydrous tetrahydrofuran and 2.53 g of pyridine, and the resulting mixture was stirred at room temperature for 3.5 hours. At the end of this time, 12.5 g of pyridine and 9.8 g of acetic anhydride were added, whilst ice-cooling, and the mixture was allowed to stand at room temperature for 1 day, after which the solvent was removed by distillation under reduced pressure, and the residue was mixed with water and then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure, to give the title compound having an Rf=0.71 (thin layer chromatography over silica gel, using a 1:1 by volume mixture of ethyl acetate and hexane as the developing solvent).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05635534 |
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| 출처 데이터셋 | uspto-grants-1997_06 |
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| ORD ID | ord-266619b5363e4d0ca8442092972ac2c5 |
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| 출처 메모 | uspto-grants-1997_06 |
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