Hydrochloric Acid → 2-Chloropyridine-3-carboxaldehyde oxime

HRID 1823263노트

반응식

HRID 1823263 반응식
[Cl:1][C:2]1[C:7]([CH:8]=O)=[CH:6][CH:5]=[CH:4][N:3]=1.Cl.[NH2:11][OH:12].[OH-].[Na+].Cl>C(O)C.O>[Cl:1][C:2]1[C:7]([CH:8]=[N:11][OH:12])=[CH:6][CH:5]=[CH:4][N:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 7376072-Chloro-3-pyridinecarboxaldehyde

생성물 1

HCID 27634542-Chloropyridine-3-carboxaldehyde oxime수율 91.1%

시약·촉매·용매 1

HCID 19096565Water ethanol용매

실험 절차

Combine 2-chloropyridine-3-carboxaldehyde (2.75 g, 0.0195 mol) with hydroxylamine hydrochloride (1.38 g, 0.021 mol) and ice (40 g) in an ethanol/water (15 mL/15 mL) mixture. Add aqueous sodium hydroxide (1.95 g, 0.049 mol, in 5 mL of water) dropwise and stir for 2.5 h near ambient temperature. Adjust the mixture to approx. pH 7.0 with aqueous hydrochloric acid, allowing for product precipitation. Extract with diethyl ether and wash with water and dry over sodium sulfate. Concentrate to obtain the desired crude oxime (2.78 g, 91%) as a white solid. MS(EI): (M)+ 156.3, 158.3 m/z.

후처리

  1. customallowing for product precipitation
  2. extractionExtract with diethyl ether
  3. washwash with water
  4. dry with materialdry over sodium sulfate
  5. concentrationConcentrate

출처 및 근거

ORD 기록
ord-b6d96089485d48ce907631b45467d6ff
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07037921B2

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