참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 5-Acetoxy-4,6-di-tert-butylbenzofuran | HCID 11822332 | — |
| 생성물 | 5-Acetoxy-4,6-di-tert-butyl-2-formylbenzofuran | HCID 22918669 | 86% |
반응 단계
Phosphorus oxychloride (1.1 g) was added dropwise to N,N-dimethylformamide (0.4 g) under cooling with ice and, subsequently, a solution of 5-acetoxy-4,6-di-tert-butylbenzofuran (1.0 g) in N,N-dimethylformamide (2 ml) was added dropwise. The mixture was stirred first at room temperature for 20 min, then under heating at 80° C. for 75 min. After cooling, the reaction mixture was poured into water and subjected to extraction ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated. The concentrate was purified by silica gel chromatography (10% ethyl acetate in n-hexane) to afford 5-acetoxy-4,6-di-tert-butyl-2-formylbenzofuran [0.95 g (yield, 86%)] as a colorless, fine-grained crystal.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05574178 |
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| 출처 데이터셋 | uspto-grants-1996_11 |
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| ORD ID | ord-c88de32d11294de09695eac5ba48c948 |
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| 출처 메모 | uspto-grants-1996_11 |
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