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Benzoic acid, 2,5-dichloro-4-fluoro- → HCID 54012777, 화합물

HRID 849259
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HRID 849259 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([Cl:12])=[CH:7][C:3]=1[C:4](O)=[O:5]>C1COCC1>[Cl:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([Cl:12])=[CH:7][C:3]=1[CH2:4][OH:5]
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참가 물질

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반응물 1

HCID 22320318Benzoic acid, 2,5-dichloro-4-fluoro-

생성물 1

HCID 54012777HCID 54012777, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 2,5-dichloro-4-fluorobenzoic acid (4.1 g, 19.6 mmol; prepared as described in the literature: Feit, P. W. et al, J. Med. Chem. 1972, Vol. 15, 79-83) in 100 mL THF was treated with 24.5 mL borane methylsulfide complex in THF (2M, 24.5 mL, 49 mmol) at 0-5° C. The mixture was allowed to come to RT, stirred for 14 h at RT and quenched by adding saturated NaHCO3 and 10 mL MeOH. The mixture was extracted with ethyl acetate, the organic layer was washed sequentially with 10% HCl and saturated NaHCO3 solutions, dried over magnesium sulfate and concentrated to give 3.65 g of the title compound as a white solid. ##STR265##

후처리

  1. customprepared
  2. customto come to RT
  3. customquenched
  4. additionby adding saturated NaHCO3 and 10 mL MeOH
  5. extractionThe mixture was extracted with ethyl acetate
  6. washthe organic layer was washed sequentially with 10% HCl and saturated NaHCO3 solutions
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f7a598d27dfb447e8642a97179aebb7f
출처 데이터셋
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06011059

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