Hydrochloric Acid → HCID 43413487, 화합물

HRID 1022583노트

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HRID 1022583 반응식
[Mg].Br[C:3]1[CH:8]=[CH:7][C:6]([Cl:9])=[C:5]([Cl:10])[CH:4]=1.[CH3:11][O:12][C:13]1[CH:22]=[CH:21][C:16]([O:17][CH2:18][C:19]#N)=[CH:15][CH:14]=1.Cl.C([O:26]CC)C>II>[Cl:10][C:5]1[CH:4]=[C:3]([C:19](=[O:26])[CH2:18][O:17][C:16]2[CH:21]=[CH:22][C:13]([O:12][CH3:11])=[CH:14][CH:15]=2)[CH:8]=[CH:7][C:6]=1[Cl:9]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 3283Diethyl Ether4회HCID 290134-Bromo-1,2-dichlorobenzeneHCID 5794914-MethoxyphenoxyacetonitrileHCID 5462224Magnesium

생성물 1

HCID 43413487HCID 43413487, 화합물

시약·촉매·용매 1

HCID 807Iodine촉매

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온도
35 °C

실험 절차

To a solution of magnesium (2.23 g) and iodine (5 mg) in diethyl ether (20 mL) was added dropwise a solution of 1-bromo-3,4-dichlorobenzene (20.7 g) in diethyl ether (20 ml), and the mixture was stirred at 35° C. for 1 hr. The reaction mixture was cooled to −10° C., and diethyl ether (100 mL) was added. A solution of (4-methoxyphenoxy)acetonitrile (10 g) in diethyl ether (20 ml) was added dropwise at −10° C., and the mixture was stirred for 1 hr while warming to room temperature. To the reaction mixture was added 1 N aqueous HCl solution (200 ml), and the mixture was stirred at room temperature for 1 hr, and extracted with ethyl acetate. The obtained extract was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (15.6 g).

후처리

  1. temperatureThe reaction mixture was cooled to −10° C.
  2. stirringthe mixture was stirred for 1 hr
  3. temperaturewhile warming to room temperature
  4. stirringthe mixture was stirred at room temperature for 1 hr
  5. extractionextracted with ethyl acetate
  6. extractionThe obtained extract
  7. washwas washed with water and brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe solvent was evaporated under reduced pressure
  10. customThe obtained residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-33b59623f2c745a086f2513e3bdf40fb
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722662B2

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