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Hydrochloric Acid → HCID 57713314, 화합물

HRID 1983860
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HRID 1983860 반응식
B(Br)(Br)Br.[F:5][C:6]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[C:9]([N+:16]([O-:18])=[O:17])=[CH:8][C:7]=1[O:19]C.O.Cl>ClCCl>[F:5][C:6]1[CH:11]=[C:10]([C:12]([F:14])([F:15])[F:13])[C:9]([N+:16]([O-:18])=[O:17])=[CH:8][C:7]=1[OH:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 25134Boron tribromideHCID 57713306HCID 57713306, 화합물

생성물 1

HCID 57713314HCID 57713314, 화합물수율 38%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 1N solution of boron tribromide in dichloromethane (15 ml) was added dropwise to a solution of 1-fluoro-2-methoxy-4-nitro-5-(trifluoromethyl)benzene obtained in Reference Example 16 (1.4 g) in dichloromethane (5 ml) with ice-cooling. After stirring at room temperature overnight, water and 1N hydrochloric acid was added to the reaction mixture. After stirring for 30 minutes, an organic layer was separated, washed with water, dried over magnesium sulfate, and concentrated. The residue was purified by column chromatography (developing solvent:ethyl acetate-hexane=1:3) to obtain the title compound as crystals (0.5 g, 38%).

후처리

  1. temperaturecooling
  2. stirringAfter stirring for 30 minutes
  3. customan organic layer was separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography (developing solvent:ethyl acetate-hexane=1:3)

출처 및 근거

ORD 기록
ord-7dde0b826aaa4501b92bb483b55f7d13
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07541478B2

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