Hydroxyamine hydrochloride → 4-Fluoro-naphthalene-1-carbaldehyde oxime

HRID 388375ノート

反応式

HRID 388375 の反応式
C([O-])(=O)C.[Na+].Cl.[NH2:7][OH:8].[F:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([CH:20]=O)=[CH:12][CH:11]=1>C1COCC1.O>[F:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:13]([CH:20]=[N:7][OH:8])=[CH:12][CH:11]=1

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 70225244-Fluoronaphthalene-1-carbaldehyde

生成物 1

HCID 866581594-Fluoro-naphthalene-1-carbaldehyde oxime

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Sodium acetate (4.8 g) is added to a solution of hydroxylamine hydrochloride (2.9 g) and 4-fluoro-naphthalene-1-carbaldehyde (8.1 g, example 1 step B) in THF (40 ml) and water (10 ml). After 3 hours at room temperature, the reaction is quenched with water and ethyl acetate. The organic, phase is separated and the water phase is extracted with ethyl acetate. The combined organic phases are washed with water and with a saturated aqueous solution of NaCl, dried over Mg2SO4 and concentrated in vacuo to yield 4-fluoro-naphthalene-1-carbaldehyde oxime. The crude product obtained is used without further purification.

後処理

  1. customthe reaction is quenched with water and ethyl acetate
  2. customThe organic, phase is separated
  3. extractionthe water phase is extracted with ethyl acetate
  4. washThe combined organic phases are washed with water and with a saturated aqueous solution of NaCl
  5. dry with materialdried over Mg2SO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3b266ea26e3643ad97a7c9fef3778853
出典データセット
uspto-grants-2013_02
特許番号
US08377942B2

反応ノート

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