Sodium Hydroxide → 2,2-Difluoro-5-methoxy-1-pentanal oxime

HRID 568981

反応式

HRID 568981 の反応式
O.[F:2][C:3]([F:11])([CH2:6][CH2:7][CH2:8][O:9][CH3:10])[CH:4]=O.[OH:12][NH:13]Cl.[OH-].[Na+].O1CCOCC1>[Cl-].[Na+].O.C(Cl)(Cl)(Cl)Cl.CCOCC>[F:2][C:3]([F:11])([CH2:6][CH2:7][CH2:8][O:9][CH3:10])[CH:4]=[N:13][OH:12]

参加物

8

反応物 4

HCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 149953Hydroxylamine, N-chloro-HCID 20149453HCID 20149453、化合物

生成物 1

HCID 736640532,2-Difluoro-5-methoxy-1-pentanal oxime収率 91%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 5943Carbon Tetrachloride溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

A mixture of 2,2-difluoro-5-methoxy-1-pentanal hydrate (1.57 g, 9.2 mmoles), hydroxylamino hydrochloride (640 mg, 9.2 mmoles), 1N NaOH (9.2 ml), and dioxane (15 ml) is kept for 1 hour at room temperature. After addition of ether and brine, usual extraction gives an oil which according to NMR is the oxime hydrate. Several evaporations with carbon tetrachloride (50° C., 60 mm Hg) afford the oxime (1.4 g) which is purified by chromatography on silica (ethyl acetate/petroleum ether: 20/80, RF: 0.53): 1.05 g (68%).

後処理

  1. customgives an oil which

出典と根拠

ORDレコード
ord-cdffc9b431c346c79072bd402f130673
出典データセット
uspto-grants-1988_03
特許番号
US04730006

関連ノート

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