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Chloromethyl Methyl Ether → HCID 90423535, 화합물

HRID 2272504
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HRID 2272504 반응식
Cl[CH2:2][O:3][CH3:4].[Br:5][C:6]1[C:7]([F:13])=[C:8]([OH:12])[CH:9]=[CH:10][CH:11]=1.C(N(CC)C(C)C)(C)C>C1COCC1>[Br:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:2][O:3][CH3:4])[C:7]=1[F:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 184012573-Bromo-2-fluorophenol

생성물 1

HCID 90423535HCID 90423535, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Chloro(methoxy)methane (11.8 mL) was added at 0 C to a THF (150 mL) solution of 3-bromo-2-fluorophenol (15.0 g) and N,N-diisopropylethylamine (41.1 mL). The reaction mixture was stirred overnight at room temperature in a nitrogen atmosphere and then filtered through celite. The obtained filtrate was washed with 1 M hydrochloric acid and a saturated aqueous solution of sodium bicarbonate in this order, and then, the solvent was distilled off under reduced pressure. The obtained residue was passed through a short silica gel column (NH, hexane/ethyl acetate), and the solvent was distilled off under reduced pressure to obtain the title compound (17.9 g)

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후처리

  1. filtrationfiltered through celite
  2. washThe obtained filtrate was washed with 1 M hydrochloric acid
  3. distillationa saturated aqueous solution of sodium bicarbonate in this order, and then, the solvent was distilled off under reduced pressure
  4. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-854e09fe67fe4a69b872eb500c56c3f6
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09120777B2

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