참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Benzene, 2-chloro-1,5-dinitro-3-(trifluoromethyl)- | HCID 67851 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 반응물 | 2,2-Difluoro-1,3-dioxaindan-4-amine | HCID 2736891 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 19103277 | HCID 19103277 | — |
반응 단계
20.8 g of LiOH.H2O are added at 0° C. to a solution of 24.5 g of 2,2-difluoro-4-amino-1,3-benzodioxole in 70 ml of dimethyl sulfoxide. The mixture is then stirred for 20 minutes. Subsequently, a solution of 38.3 g of 2,4-dinitro-6-trifluoromethylchlorobenzene in 70 ml of dimethyl sulfoxide is added, and the resultant reaction mixture is stirred at 0° C. for 20 minutes and then heated to room temperature. After 5 hours, the mixture is poured into 350 ml of water, acidified with dilute hydrochloric acid and extracted several times with diethyl ether. The combined ether phases are washed three times with a 5% solution of sodium carbonate and then with 5% hydrochloric acid and dried over sodium sulfate, and the solvent is evaporated off in vacuo. The residue comprises 51.6 g of orange-brown crystals which are recrystallised in toluene. Yield: 41.6 g; melting point: 144°-146° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04722935 |
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| 출처 데이터셋 | uspto-grants-1988_02 |
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| ORD ID | ord-c71b9f3cdcad49d1b3a53a42a03aed7c |
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| 출처 메모 | uspto-grants-1988_02 |
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