化工社化工社 化学情報印刷レポート · 研究参考用
Water → Xilobam
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,6-Xylyl isocyanate | HCID 98787 | — |
| 反応物 | 1-Methylpyrrolidin-2-imine hydrochloride | HCID 12448967 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Xilobam | HCID 39689 | — |
反応手順
To a stirring solution of 6.73 g. (0.05 mole) of 1-methyl- 2-iminopyrrolidine hydrochloride in about 2 ml. of water is added about 50 ml. of benzene followed by 10 ml. of 50% NaOH. After stirring 1 min. the benzene layer is decanted onto anhydrous potassium carbonate. The extraction is repeated twice. The combined benzene extracts are filtered from a drying agent (dicalite pad) and rinsed well with dry benzene. To the filtrate is added in one portion with stirring 7.36 g. (0.05 mole) of 2,6-dimethylphenylisocyanate. The reaction mixture is stirred overnight. Solvent removal and recrystallization from ethyl acetate-ether gives the product, 1-(2,6 -dimethylphenyl)-3-(1-methyl-2-pyrrolidylidene)urea, as white crystals, m.p. = 119°-120° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03998958 |
| 出典データセット | uspto-grants-1976_12 |
| ORD ID | ord-c9c45004406b44bfbb0dfc6151186571 |
| 出典メモ | uspto-grants-1976_12 |