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Butylurea → N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butylurea | HCID 11595 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-[2-(1-Oxo-isoindoline-2-carboxamido)-ethyl]-benzene sulfochloride | HCID 21162349 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzenesulfonyl)-N'-butyl-urea | HCID 21162325 | — |
反応手順
4.8 g of butyl urea are dissolved in 100 ml of tetrahydrofurane and, while stirring, 1.5 g of 80% sodium hydride (in oil) are added. The mixture is heated for 3 hours to 60° C. whereupon 7.6 g of 4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]-benzene-sulfochloride in 100 ml of tetrahydrofurane are added while cooling. The temperature is slowly raised to 60°-70° C. and stirring is continued at that temperature for 3 hours. The solvent is removed under reduced pressure, water is added to the residue, the mixture is filtered and the filtrate is acidified with dilute hydrochloric acid. After recrystallization from dilute acetone, the N-(4-[2-(1-oxo-isoindoline-2-carboxamido)-ethyl]benzenesulfonyl)-N'-butyl-urea melts at 189°-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04282239 |
| 出典データセット | uspto-grants-1981_08 |
| ORD ID | ord-eeaef196eedc4b268efebd985dfcd232 |
| 出典メモ | uspto-grants-1981_08 |