참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | 2,4-Di-tert-butylphenol | HCID 7311 | — |
| 반응물 | 3-(4-Allyloxyphenyl)-5,7-di-tert-butylbenzofuran-2-one | HCID 19930565 | — |
| 생성물 | 3-(2,2-Dimethyldihydrobenzofuran-5-yl)-5,7-di-tert-butylbenzofuran-2-one | HCID 70272430 | 20% |
반응 단계
A mixture of 20.6 g (0.10 mol) of 2,4-di-tert-butylphenol and 22.6 g (0.10 mol) of 4-methallyloxymandelic acid (preparation as in Example 1) is kept at 155° C. under reduced pressure (50 mbar) for 8 hours. The reaction mixture is then heated to 220° C. under nitrogen and kept at this temperature for about 100 minutes. After cooling to about 120° C., 100 ml of acetic acid and 2 ml of methanesulfonic acid are added and the solution is refluxed for 3 hours. The reaction mixture is cooled, and the product is precipitated with 10 ml of ethanol and isolated by filtration. Recrystallisation from ethanol (100 ml)/acetic acid (8 ml) gives 8.0 g (20%) of 3-(2,2-dimethyldihydrobenzofuran-5-yl)-5,7-di-tert-butylbenzofuran-2-one, m.p. 164°-166° C. (compound (102), Table 1 ).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05428177 |
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| 출처 데이터셋 | uspto-grants-1995_06 |
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| ORD ID | ord-7c22e702c69b48c5a3d0cfb18b638bfb |
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| 출처 메모 | uspto-grants-1995_06 |
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