참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 2-Aminomethyl-1-ethylpyrrolidine | HCID 117295 | — |
| 반응물 | 3,5-Dichloro-2,6-dimethoxybenzoic Acid | HCID 2774750 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Benzamide, 3,5-dichloro-2,6-dimethoxy-N-(1-ethyl-2-pyrrolidinylmethyl)- | HCID 54941 | — |
반응 단계
20 ml of thionyl chloride is added to 11.9 g (0.047 mol) of 3,5-dichloro-2,6-dimethoxybenzoic acid. The mixture is heated on a steam bath for 30 minutes. To the solution is added 50 ml of toluene. The solvent and excess thionyl chloride is evaporated at reduced pressure. The residue is dissolved in 50 ml of dry ethyl ether. To the obtained solution is added dropwise while stirring 6.0 g (0.047 mol) of 2-(aminomethyl)-1-ethylpyrrolidine in 50 ml of ethyl ether. After 30 minutes at room temperature 300 ml of water is added while stirring. The water layer is separated and alkalized with sodium hydroxide solution which is added dropwise while stirring and cooling in ice. The precipitate is collected and washed with water. Yield: 9.0 g, m.p. 120°-21° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04232037 |
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| 출처 데이터셋 | uspto-grants-1980_11 |
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| ORD ID | ord-b3b738a827e8417e8e72b8888fb1ea24 |
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| 출처 메모 | uspto-grants-1980_11 |
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