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O-tert-butylhydroxylamine hydrochloride → (E)-2-(3-bromo-alpha-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine

HRID 442735
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HRID 442735 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][C:16]=1[F:17])[C:5]([C:7]1[C:12]([OH:13])=[CH:11][CH:10]=[CH:9][N:8]=1)=O.Cl.[C:19]([O:23][NH2:24])([CH3:22])([CH3:21])[CH3:20]>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][C:16]=1[F:17])/[C:5](/[C:7]1[C:12]([OH:13])=[CH:11][CH:10]=[CH:9][N:8]=1)=[N:24]\[O:23][C:19]([CH3:22])([CH3:21])[CH3:20].[Br:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][C:16]=1[F:17])/[C:5](/[C:7]1[C:12]([OH:13])=[CH:11][CH:10]=[CH:9][N:8]=1)=[N:24]/[O:23][C:19]([CH3:22])([CH3:21])[CH3:20]
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참가 물질

5

반응물 2

HCID 2777906O-tert-butylhydroxylamine hydrochlorideHCID 539533172-(3-Bromo-4-fluorobenzoyl)-3-hydroxypyridine

생성물 2

HCID 135494341(E)-2-(3-bromo-alpha-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridineHCID 136340705(Z)-2-(3-bromo-alpha-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
90 °C

실험 절차

A mixture of 2-(3-bromo-4-fluorobenzoyl)-3-hydroxypyridine (2.96 g), O-t-butyl hydroxylamine hydrochloride (1.88 g) and acetic acid (50 mL) was stirred at 90° C. for 14 hours. The reaction mixture was concentrated in vacuo, which was subjected to addition with ethyl acetate and water. The ethyl acetate solution was washed with aqueous NaHCO3 and a saturated aqueous saline solution, successively, which was dried (magnesium sulfate), followed by distilling off the solvent under reduced pressure. The residue was subjected to purification by means of a silica gel column (ethyl acetate--hexane) to afford (E)-2-(3-bromo-α-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine (1.10 g) and (Z)-2-(3-bromo-α-t-butoxyimino-4-fluorobenzyl)-3-hydroxypyridine (1.97 g) (compounds 17 and 16).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo, which
  2. additionwas subjected to addition with ethyl acetate and water
  3. washThe ethyl acetate solution was washed with aqueous NaHCO3
  4. dry with materiala saturated aqueous saline solution, successively, which was dried (magnesium sulfate)
  5. distillationby distilling off the solvent under reduced pressure
  6. customThe residue was subjected to purification by means of a silica gel column (ethyl acetate--hexane)

출처 및 근거

ORD 기록
ord-060eb891c1b04e35bbda8a1fb4ae6123
출처 데이터셋
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05891895

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