Hydroxyamine hydrochloride → N-[(2,4-dichloro-1,3-thiazol-5-yl)methylidene]hydroxylamine

HRID 1584025노트

반응식

HRID 1584025 반응식
Cl.[NH2:2][OH:3].[Cl:4][C:5]1[S:6][C:7]([CH:11]=O)=[C:8]([Cl:10])[N:9]=1.C(=O)(O)[O-].[Na+]>C(O)C.O>[Cl:4][C:5]1[S:6][C:7]([CH:11]=[N:2][OH:3])=[C:8]([Cl:10])[N:9]=1

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 14886722,4-Dichloro-1,3-thiazole-5-carboxaldehyde

생성물 1

HCID 2778786N-[(2,4-dichloro-1,3-thiazol-5-yl)methylidene]hydroxylamine수율 99%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

First 153 g (2.2 mol) of hydroxylamine hydrochloride in portions, then a solution of 364 g (2 mol) of 2,4-dichloro-5-thiazolecarboxaldehyde (II) in 1 liter of ethanol are added to a solution of 185 g (2.2 mol) of sodium bicarbonate in 5 liters of water at room temperature, with stirring. A voluminous, colourless precipitate separates out after 1 to 2 minutes. After stirring for 1 hour, the solid is filtered off with suction, washed with water and dried. 390 g (=99% of theory) of 2,4-dichloro-5-thiazolecarboxaldehyde oxime (IV) of melting point about 160° C. are obtained. It can be dehydrated to give the nitrile without further purification.

후처리

  1. stirringAfter stirring for 1 hour
  2. filtrationthe solid is filtered off with suction
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-850e7a4834c34d218b58c255fcd44d36
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04555577

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