Hydrochloric Acid → 3,5-Dichloro-4-pyridinecarbaldehyde oxime

HRID 1823284ノート

反応式

HRID 1823284 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:10])[C:7]=1[CH:8]=O.Cl.[NH2:12][OH:13].[OH-].[Na+].Cl>C(OCC)C.C(O)C.O>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:10])[C:7]=1[CH:8]=[N:12][OH:13]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 27629883,5-Dichloro-4-pyridinecarboxaldehyde

生成物 1

HCID 1363488123,5-Dichloro-4-pyridinecarbaldehyde oxime収率 98.2%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 19096565Water ethanol溶媒

実験手順

Combine 3,5-dichloropyridine-4-carboxaldehyde (2.80 g, 0.016 mol) with hydroxylamine hydrochloride (1.13 g, 0.018 mol) and ice (50 g) in an ethanol/water (30 mL/30 mL) mixture. Add aqueous sodium hydroxide (1.63 g, 0.024 mol, in 20 mL of water) dropwise and stir for 4 h near ambient temperature. Adjust the mixture to approx. pH 7.0 with aqueous hydrochloric acid and extracte with diethyl ether. Dry the combined extracts over sodium sulfate and concentrate in vacuo to give the desired crude oxime (3.00 g, 88%) as a light solid. MS(ES): (M+1)+ 190.9, 192.9 m/z.

後処理

  1. dry with materialDry the combined extracts over sodium sulfate
  2. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-e0a1c12509244b5083ccc856b89e579c
出典データセット
uspto-grants-2006_05
特許番号
US07037921B2

反応ノート

読み込み中…