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Ammonia → 3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trichloroisocyanuric Acid | HCID 6909 | — |
| 反応物 | 3-(2-Bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea | HCID 13059860 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea | HCID 67788573 | — |
反応手順
2.1 g of 3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea (5 mmol) and 388 mg of trichloroisocyanuric acid (1.67 mmol) are dissolved in 100 ml of trifluoroacetic acid at room temperature. After 15 minutes, ice is added, it is made alkaline with conc. ammonia and shaken out with dichloromethane. The organic phases are dried and concentrated by evaporation, the residue is chromatographed and the product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05411966 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-e4f87c257b9c434bb882cda9bcf99f6e |
| 出典メモ | uspto-grants-1995_05 |