Potassium Carbonate → HCID 18504682, 화합물

HRID 1356961노트

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HRID 1356961 반응식
[CH2:1]([C:3]1[CH:4]=[C:5]([OH:25])[CH:6]=[C:7]([CH3:24])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][N:15]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[Cl:32][C:33]([Cl:37])=[CH:34][CH2:35]Cl>CN(C)C=O>[CH2:1]([C:3]1[CH2:4][C:5]([CH3:6])([O:25][CH2:35][CH:34]=[C:33]([Cl:37])[Cl:32])[CH:24]=[CH:7][C:8]=1[O:9][CH2:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][N:15]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 173781,1,3-TrichloropropeneHCID 18504580HCID 18504580, 화합물

생성물 1

HCID 18504682HCID 18504682, 화합물수율 65.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

In 10 ml of N,N-dimethylformamide were dissolved 0.7 g of 3-ethyl-5-methyl-4-[3-(5-trifluoromethyl-2-pyridyloxy)propyloxy]phenol and 0.27 g of potassium carbonate, to which a solution of 0.34 g of 1,1,3-trichloropropene dissolved in 5 ml of N,N-dimethylformamide was added dropwise, while stirring at room temperature. After stirring at room temperature for 12 hours, the reaction mixture was poured into ice-water, and extracted twice with 100 ml of diethyl ether. The combined diethyl ether was washed with water, dried with anhydrous magnesium sulfate, and concentrated to obtain a crude product. The crude produce was subjected to silica gel chromatography, which afforded 0.6 g of 3-ethyl-1-methyl-4-[3-(5-trifluoromethyl-2-pyridyloxy)propyloxy]-1-(3,3-dichloro-2-propenyloxy)benzene (65% yield), nD23.0 1.5188.

후처리

  1. additionwas added dropwise
  2. stirringAfter stirring at room temperature for 12 hours
  3. extractionextracted twice with 100 ml of diethyl ether
  4. washThe combined diethyl ether was washed with water
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto obtain a crude product
  8. customThe crude produce

출처 및 근거

ORD 기록
ord-46d53f49a0924a44a1d208a1755702f5
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06589914B2

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