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4-Chloroaniline → LY 181984
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloroaniline | HCID 7812 | — |
| 反応物 | p-Toluenesulfonyl isocyanate | HCID 77703 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | LY 181984 | HCID 160725 | 94.3% |
反応手順
A solution of 6.25 g (49.00 mmoles) of 4-chloroaniline in 10 ml of methylene chloride was added to a solution of 9.85 g (49.95 mmoles) of p-toluenesulfonyl isocyanate in 75 ml of methylene chloride with stirring. The mixture became quite warm and a heavy white precipitate formed. An additional 100 ml of methylene chloride were added. The reaction mixture was stirred an additional 15 minutes, and the precipitate was recovered by filtration affording 15.0 g of the title product as a white solid. A small amount of the material was crystallized from diethyl ether to provide the title compound (87% yield) with a melting point of 174-176_C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06281240B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-1760152cf4e848c6a7a57f68ac077b82 |
| 出典メモ | uspto-grants-2001_08 |