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

HRID 1823284노트

반응식

HRID 1823284 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 1363488123,5-Dichloro-4-pyridinecarbaldehyde oxime수율 98.2%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 19096565Water ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e0a1c12509244b5083ccc856b89e579c
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07037921B2

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