반응식
[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:3]=1[CH2:4][O:5][CH2:6][CH2:7][OH:8].C(N(CC)CC)C.[F:21][C:22]([F:43])([F:42])[C:23]1[CH:41]=[CH:40][C:26]([O:27][C:28]2[CH:39]=[CH:38][C:31]([O:32][CH:33]([CH3:37])[C:34](Cl)=[O:35])=[CH:30][CH:29]=2)=[CH:25][CH:24]=1>C1(C)C=CC=CC=1>[F:21][C:22]([F:42])([F:43])[C:23]1[CH:41]=[CH:40][C:26]([O:27][C:28]2[CH:39]=[CH:38][C:31]([O:32][CH:33]([CH3:37])[C:34]([O:8][CH2:7][CH2:6][O:5][CH2:4][C:3]3[C:2]([Cl:1])=[CH:12][CH:11]=[CH:10][C:9]=3[Cl:13])=[O:35])=[CH:30][CH:29]=2)=[CH:25][CH:24]=1참가 물질
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- 온도
- 0 °C
실험 절차
22.1 g of 2-(2,6-dichlorobenzyloxy)ethanol and 10.1 g of triethylamine were dissolved in 200 ml of toluene, then cooled to 0° C. To this solution was dropwise added a solution of 34.5 g of 2-[4-(4-trifluoromethylphenoxy)phenoxy]propionyl chloride in 50 ml of toluene at 0° to 10° C. After the dropwise addition, the reaction mixture was gradually heated and, at 40° C., it was stirred for one hour to complete the reaction. After cooling the reaction solution to room temperature, it was washed successively with 1% strength by weight sodium hydroxide aqueous solution and water, then dehydrated. After distilling off toluene under reduced pressure, the resulting colorless, viscous, oily product was allowed to stand for about 1 month to obtain 49.2 g of crystalline 2-(2,6-dichlorobenzyloxy)ethyl 2-[4-(4-trifluoromethylphenoxy)phenoxy]propionate. m.p. 51° to 53° C.
후처리
- additionAfter the dropwise addition
- temperaturethe reaction mixture was gradually heated and, at 40° C.
- customthe reaction
- temperatureAfter cooling the reaction solution to room temperature
- washit was washed successively with 1% strength by weight sodium hydroxide aqueous solution and water
- distillationAfter distilling off toluene under reduced pressure
- waitto stand for about 1 month
출처 및 근거
- ORD 기록
- ord-81c65e9b7c0842f0b1004984e7e6694b
- 출처 데이터셋
- uspto-grants-1984_04
- 특허 번호
- US04441913
연결된 노트
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