참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl Sulfide | HCID 1068 | — |
| 반응물 | Butyl nitrite | HCID 10996 | — |
| 반응물 | 2-(4,5-Dihydroisoxazol-3-yl)-3-methylaniline | HCID 9794006 | — |
| 촉매 | Cuprous chloride | HCID 62652 | — |
| 생성물 | 3-(2-Methyl-6-methylthiophenyl)-4,5-dihydroisoxazole | HCID 10878342 | — |
반응 단계
40 g (0.22 mol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline and 0.44 g of copper(I) chloride are initially charged in 300 ml of dimethyl sulfide, and 26.1 g of n-butyl nitrite (0.23 mol) are added dropwise at 55-66° C. The mixture is then stirred at 60° C. for 1.5 hours. For work-up, the mixture is then washed with dilute hydrochloric acid and water and then concentrated under reduced pressure. This gives 38.7 g (85%) of a dark oil which solidifies after a while (content according to HPLC 94%). The product can be purified further by trituration in methyl tert-butyl ether.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06706886B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-eebd678ebf0344898ce01b01fd0724f3 |
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| 출처 메모 | uspto-grants-2004_03 |
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