関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | 6-(2-hydroxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran | HCID 18782888 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(2-tert-butyidimethylsilyloxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran | HCID 54380817 | 94% |
反応手順
6-(2-hydroxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran (1.1 g) (see Preparation 10) was dissolved in dry dimethylformamide (2 ml) and imidazole (0.55 g) and tert-butyidimethylsilyl chloride (0.61 g) were added. The flask was fitted with a calcium chloride drying tube and the mixture stirred at 40° C for 90 minutes. Water was added and the mixture was extracted with diethyl ether. The organic extract was washed with aqueous sodium hydrogen carbonate solution (×2), dried (anhydrous sodium sulphate), the solvent removed under reduced pressure and the crude product was chromatographed on silica using 4:1 hexane:dichloromethane as the eluent to yield 6-(2-tert-butyldimethylsilyloxyphenyl)thio-2,2,3-trimethyl-2H-benzo[b]pyran (1.43 g) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06071938 |
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| 出典データセット | uspto-grants-2000_06 |
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| ORD ID | ord-c6cf635cea654da794d69a5f7a88b482 |
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| 出典メモ | uspto-grants-2000_06 |
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