化工社化工社 化学情報印刷レポート · 研究参考用
1,1-Dimethylhydrazine → N-dimethylamino-3-chloro-2,6-dinitro-4-trifluoromethylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1-Dimethylhydrazine | HCID 5976 | — |
| 反応物 | 2,4-Dichloro-1,3-dinitro-5-(trifluoromethyl)benzene | HCID 94398 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | N-dimethylamino-3-chloro-2,6-dinitro-4-trifluoromethylaniline | HCID 13101276 | 85% |
反応手順
To 20.0 g. (0.065 mole) of 2,4-dichloro-3,5-dinitrobenzotrifluoride and 300 ml. of cyclohexane in a 500 ml. roundbottom flask equipped with a stirrer and dropping funnel was added 7.86 g. (0.13 mole) of 1,1-dimethylhydrazine at ambient temperature. The addition was drop-wise over a period of about 20 minutes. Stirring was continued for 22 hours at room temperature. The resultant mixture was filtered and the insoluble solid then stirred with 300 ml. of water for one hour to dissolve the hydrazine hydrochloride. The insoluble product was isolated by filtration and washed with water. Recrystallization from 95% ethanol gave 18.3 g. (85%) of the desired product as a yellow solid, m.p. 130° - 131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04138244 |
| 出典データセット | uspto-grants-1979_02 |
| ORD ID | ord-0129388f688e4c64a9074135c36c8b99 |
| 出典メモ | uspto-grants-1979_02 |