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Hydroxyamine hydrochloride → 2-Chloro-6-fluoro-4-hydroxybenzonitrile

HRID 2178137
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HRID 2178137 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([OH:10])[CH:7]=[C:6]([F:11])[C:3]=1[CH:4]=O.Cl.[NH2:13]O.C([O-])=O.[Na+]>C(O)=O>[Cl:1][C:2]1[CH:9]=[C:8]([OH:10])[CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:13]
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참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 2723810Sodium FormateHCID 584026032-Chloro-6-fluoro-4-hydroxybenzaldehyde

생성물 1

HCID 1176531442-Chloro-6-fluoro-4-hydroxybenzonitrile수율 56%

시약·촉매·용매 1

HCID 284Formic Acid용매

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온도
105 °C

실험 절차

A solution of 2-chloro-6-fluoro-4-hydroxybenzaldehyde (WO 2008141249, 90 mg, 0.344 mmol) in formic acid (1 mL) was treated with hydroxylamine hydrochloride (23.9 mg, 0.344 mmol) and sodium formate (23.4 mg, 0.344 mmol) and stirred under nitrogen for 3.5 hours at 105° C. The mixture was concentrated in vacuo and the residue treated with saturated aqueous sodium bicarbonate solution (10 mL). The aqueous solution was extracted with ethyl acetate (2×10 mL), dried over sodium sulphate and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 30-50% EtOAc in heptanes to afford the title compound as a beige solid (33 mg, 56%).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. additionthe residue treated with saturated aqueous sodium bicarbonate solution (10 mL)
  3. extractionThe aqueous solution was extracted with ethyl acetate (2×10 mL)
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified
  7. washeluting with 30-50% EtOAc in heptanes

출처 및 근거

ORD 기록
ord-7c4afb027058457f87d1ff26f687dcdf
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09067922B2

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