関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,6-Trivinylboroxin-Pyridine Complex | HCID 2734806 | — |
| 反応物 | 3-Chloro-6,7-dihydro[1,4]oxathiino[3,2-c]pyridazine | HCID 86623079 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 3-Ethenyl-6,7-dihydro[1,4]oxathiino[3,2-c]pyridazine | HCID 67527273 | 71.2% |
反応手順
A solution of 3-chloro-6,7-dihydro[1,4]oxathiino[3,2-c]pyridazine (450 mg, 2.4 mmol) in dimethoxyethane (12 ml) was treated with tetrakis(triphenylphosphine)palladium (0) (61 mg), potassium carbonate (313 mg), 2,4,6-trivinylcyclotriboroxane pyridine complex (375 mg) and water (1.5 ml). The mixture was heated at 96° C., overnight. The mixture was evaporated to dryness, treated with aqueous sodium bicarbonate solution, extracted (4×) with DCM, dried (sodium sulphate), evaporated and chromatographed on silica gel (50 g), eluting with 1:1 ethyl acetate-hexane, affording a solid (200 mg, 46%), containing slightly impure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07732460B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-ddbc66b9b4ed49d5bcddcc05649432f6 |
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| 出典メモ | uspto-grants-2010_06 |
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