関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,2-Dimethoxyethylmethylamine | HCID 8503 | — |
| 反応物 | 4-Chloro-3,5-dinitrobenzotrifluoride | HCID 9809 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | N-Methyl-N-(2,2-dimethoxyethyl)-2,6-dinitro-4-trifluoromethylaniline | HCID 20492553 | — |
反応手順
4-Chloro-3,5-dinitrobenzotrifluoride (5.4 grams; 0.02 mole) dissolved in benzene was charged into a glass reaction vessel equipped with a mechanical stirrer and addition funnel. N-Methyl-N-2,2-dimethoxyethylamine (2,4 grams; 0.02 mole) and triethylamine (2.02 grams; 0.02 mole) both dissolved in benzene (50 ml) were then added dropwise with stirring. After the addition was completed stirring was continued for a period of 1 hour resulting in the formation of a precipitate. The reaction mixture was filtered to remove the acid acceptor salt and was chromatographed. The solution was then evaporated to yield a solid product. This solid was recrystallized from hexane to yield the desired product N-methyl-N-(2,2-dimethoxyethyl)-2,6-dinitro-4-trifluoroemethylaniline melting at 48° to 50° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04397677 |
|---|
| 出典データセット | uspto-grants-1983_08 |
|---|
| ORD ID | ord-c42d1d4d697547de80e21add2200b073 |
|---|
| 出典メモ | uspto-grants-1983_08 |
|---|