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Cornforth reagent → 3-(9,10-Didehydro-6-methyl-14-nitro-8alpha-ergolinyl)-1,1-diethylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cornforth reagent | HCID 2724130 | — |
| 反応物 | 3-(9,10-Didehydro-2,3-dihydro-6-methyl-14-nitro-8alpha-ergolinyl)-1,1-diethylurea | HCID 86742350 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(9,10-Didehydro-6-methyl-14-nitro-8alpha-ergolinyl)-1,1-diethylurea | HCID 13374959 | 46.9% |
反応手順
A solution is prepared from 150 mg of 3-(9,10-didehydro-2,3-dihydro-6-methyl-14-nitro-8α-ergolinyl)-1,1-diethylurea in 5 ml of methylene chloride; 250 mg of pyridinium dichromate, dissolved in 2 ml of methylene chloride, is added to the reaction mixture and the latter is agitated for one hour at room temperature. Then the mixture is diluted with water, extracted by shaking with methylene chloride, the organic phase is dried and evaporated. The residue is chromatographed on silica gel with methylene chloride/methanol (5%), thus obtaining 70 mg of 3-(9,10-didehydro-6-methyl-14-nitro-8α-ergolinyl)-1,1-diethylurea.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04766128 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-ccae881c61ab40a7ad74fdb1aa4f7210 |
| 出典メモ | uspto-grants-1988_08 |