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

HRID 442735
ノート
印刷プレビュー

反応式

HRID 442735 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-060eb891c1b04e35bbda8a1fb4ae6123
出典データセット
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05891895

反応ノート

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