関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,3-Dihydroxybutanedioic Acid | HCID 875 | — |
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 反応物 | 3-(12-Acetylamino-9,10-didehydro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea | HCID 86742356 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-(9,10-Didehydro-12-ethylamino-6-methyl-8alpha-ergolinyl)-1,1-diethylurea | HCID 86742355 | 70% |
反応手順
200 mg of 3-(12-acetylamino-9,10-didehydro-6-methyl-8α-ergolinyl)-1,1-diethylurea is dissolved in 10 ml of dioxane, combined with 2 ml of 20% diisobutyl aluminum hydride solution in toluene, and heated to 100° C. for 7 hours. The mixture is allowed to cool, then, under cooling, first water, thereafter 2N hydrochloric acid are added thereto, and the solution is rendered alkaline with dilute ammonia, after adding about 1 g of tartaric acid. The mixture is extracted by shaking with methylene chloride, the organic phase is dried and evaporated. The residue is charomatographed as disclosed in Example 7, thus producing 135 mg of 3-(9,10-didehydro-12-ethylamino-6-methyl-8α-ergolinyl)-1,1-diethylurea.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04766128 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-5ab883efae4c44dbb6f8600b043a3b98 |
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| 出典メモ | uspto-grants-1988_08 |
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