참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Benzoyl chloride, 3,6-dichloro-2-methoxy- | HCID 82609 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | N-Methyl-2-Methoxy-3,6-Dichlorobenzamide | HCID 14156699 | — |
반응 단계
Methylamine (146.1 grams; 4.70 moles) contained in 40% aqueous methyl amine solution (365.4 grams) was placed in a 3-liter, 3-necked glass reaction flask equipped with addition funnel, stirrer, thermometer and reflux condenser and containing ether (1200 ml) cooled to 4° C. 2-methoxy-3,6-dichlorobenzoic acid chloride (375 grams; 1.56 moles) in ether (50 ml) was added dropwise with stirring maintaining the temperature below 8° C. After the completion of the addition the reaction mixture was stirred for an additional two hours at a temperature of between 2° and 5° C. The insoluble white solid was filtered with suction, washed with water, transferred to a 3-liter beaker and stirred fifteen (15) minutes with 10% sodium carbonate (2 liters). The insoluble white solid was filtered with suction, washed with water and dried. The product weighed 352 grams and had a melting point of 172.5°-175° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04536210 |
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| 출처 데이터셋 | uspto-grants-1985_08 |
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| ORD ID | ord-19573ff6a9384c6aa70d895de30085d0 |
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| 출처 메모 | uspto-grants-1985_08 |
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