Triethylamine → 2-(2,6-Dichlorobenzyloxy)ethyl 2-[4-(4-trifluoromethylphenoxy)phenoxy]propionate

HRID 325592

反応式

HRID 325592 の反応式
[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]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 129060152-{4-[4-(Trifluoromethyl)phenoxy]phenoxy}propanoyl chlorideHCID 13341669Ethanol, 2-((2,6-dichlorophenyl)methoxy)-

生成物 1

HCID 133416702-(2,6-Dichlorobenzyloxy)ethyl 2-[4-(4-trifluoromethylphenoxy)phenoxy]propionate収率 93%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  1. additionAfter the dropwise addition
  2. temperaturethe reaction mixture was gradually heated and, at 40° C.
  3. customthe reaction
  4. temperatureAfter cooling the reaction solution to room temperature
  5. washit was washed successively with 1% strength by weight sodium hydroxide aqueous solution and water
  6. distillationAfter distilling off toluene under reduced pressure
  7. waitto stand for about 1 month

出典と根拠

ORDレコード
ord-81c65e9b7c0842f0b1004984e7e6694b
出典データセット
uspto-grants-1984_04
特許番号
US04441913

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