Potassium Carbonate → 3-Chloro-4-[3-(4-trifluoromethylphenoxy) propyloxy]-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene

HRID 363086ノート

反応式

HRID 363086 の反応式
Br[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][CH:7]=1.BrCCCOC1C=CC(OC(F)(F)F)=CC=1.C(=O)([O-])[O-].[K+].[K+].[Cl:38][C:39]1[CH:44]=[C:43]([O:45][CH2:46][CH:47]=[C:48]([Cl:50])[Cl:49])[CH:42]=[C:41]([CH3:51])[C:40]=1[OH:52]>CN(C)C=O.C(OCC)C>[Cl:38][C:39]1[CH:44]=[C:43]([O:45][CH2:46][CH:47]=[C:48]([Cl:49])[Cl:50])[CH:42]=[C:41]([CH3:51])[C:40]=1[O:52][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][CH:7]=1

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 11781023Benzene, 1-(3-bromopropoxy)-4-(trifluoromethyl)-HCID 136722751-(3-Bromopropoxy)-4-(trifluoromethoxy)benzeneHCID 185046952-Chloro-6-methyl-4-(3,3-dichloro-2-propenyloxy)phenol

生成物 1

HCID 538030523-Chloro-4-[3-(4-trifluoromethylphenoxy) propyloxy]-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene収率 94.9%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

First, 0.35 g of 1-(3-bromopropyloxy)-4-trifluoromethylbenzene (prepared in the same manner as described above for 1-(3-bromopropyloxy)-4-trifluoromethoxybenzene) and 0.2 g of potassium carbonate were dissolved in 100 ml of N,N-dimethylformamide, to which 0.3 g of 2-chloro-6-methyl-4-(3,3-dichloro-2-propenyloxy)phenol was added, and the mixture was stirred at room temperature for 24 hours. The reaction mixture was mixed with 200 ml of diethyl ether, washed with water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude product was subjected to silica gel chromatography, which afforded 0.50 g of 3-chloro-4-[3-(4-trifluoromethylphenoxy) propyloxy]-5-methyl-1-(3,3-dichloro-2-propenyloxy)benzene (94% yield), nD23.0 1.5330.

後処理

  1. additionwas added
  2. washwashed with water
  3. dry with materialdried with anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customto obtain a crude product

出典と根拠

ORDレコード
ord-ea71162892f44dcabd4cc1a971eff7e4
出典データセット
uspto-grants-1999_02
特許番号
US05872137

反応ノート

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