Potassium Carbonate → 2,5-Dichloro-4-(3-bromo-5-trifluoromethyl-2-pyridyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene

HRID 260776

반응식

HRID 260776 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[C:14]([Br:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][N:10]=2)[C:5]([Cl:20])=[CH:4][C:3]=1[OH:21].C(=O)([O-])[O-].[K+].[K+].[Cl:28][C:29]([Cl:33])=[CH:30][CH2:31]Cl>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[C:14]([Br:15])=[CH:13][C:12]([C:16]([F:17])([F:19])[F:18])=[CH:11][N:10]=2)[C:5]([Cl:20])=[CH:4][C:3]=1[O:21][CH2:31][CH:30]=[C:29]([Cl:33])[Cl:28]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 173781,1,3-TrichloropropeneHCID 214663082,5-Dichloro-4-(3-bromo-5-trifluoromethyl-2-pyridyloxy)phenol

생성물 1

HCID 214663982,5-Dichloro-4-(3-bromo-5-trifluoromethyl-2-pyridyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene수율 83%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a mixture of 0.77 g of 2,5-dichloro-4-(3-bromo-5-trifluoromethyl-2-pyridyloxy)phenol, 0.29 g of potassium carbonate and 20 ml of N,N-dimethylformamide, a solution prepared by dissolving 0.31 g of 1,1,3-trichloropropene in 5 ml of N,N-dimethylformamide was added dropwise at room temperature with stirring. After stirring at room temperature for 10 hours, the reaction solution was poured into ice-water, and extracted twice with 50 ml of ethyl acetate. Then, the ethyl acetate layers were combined, washed with water, dried over anhydrous magnesium sulfate and then concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 0.81 g of 2,5-dichloro-4-(3-bromo-5-trifiuoromethyl-2-pyridyloxy)-1-(3,3-dichloro-2-propenyloxy)benzene, yield 83%; m.p., 95.4° C.

후처리

  1. customa solution prepared
  2. additionwas added dropwise at room temperature
  3. stirringAfter stirring at room temperature for 10 hours
  4. extractionextracted twice with 50 ml of ethyl acetate
  5. washwashed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. customto give a crude product

출처 및 근거

ORD 기록
ord-ef28b9322fc04263812c90391fac75d9
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530015

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