참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Lithium iodide | HCID 66321 | — |
| 반응물 | 6-(2-methoxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran | HCID 18782865 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| 생성물 | 6-(2-hydroxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran | HCID 18782888 | 35.9% |
반응 단계
6-(2-Methoxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran (3.5 g) (see Preparation 7) was dissolved in dry 2,4,6-collidine (15 ml), anhydrous lithium iodide (9.0 g) was added and the mixture was heated at 150° C for 40 hours. After cooling, the mixture was taken up in dichloromethane and washed with 2N aqueous hydrochloric acid solution (×3). The organic layer was dried (anhydrous sodium sulphate), the solvent removed under reduced pressure and the residue was chromatographed on silica using 1:1 hexane:dichloromethane as the eluent to yield 6-(2-hydroxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran (1.2 g) as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06071938 |
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| 출처 데이터셋 | uspto-grants-2000_06 |
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| ORD ID | ord-c2d9dbbdab2c46f6814021f0ef5c1049 |
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| 출처 메모 | uspto-grants-2000_06 |
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