Sodium Hydroxide → 5-Nitro-2-thiophenecarboxaldehyde oxime

HRID 1860268

반응식

HRID 1860268 반응식
[N+:1]([C:4]1[S:8][C:7]([CH:9]=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].Cl.[NH2:12][OH:13].[OH-].[Na+]>C(O)C.O.ClCCl>[N+:1]([C:4]1[S:8][C:7]([CH:9]=[N:12][OH:13])=[CH:6][CH:5]=1)([O-:3])=[O:2]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 782815-Nitrothiophene-2-carboxaldehydeHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 3505165-Nitro-2-thiophenecarboxaldehyde oxime수율 79.9%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 19096565Water ethanol용매

실험 절차

A mixture of 5-nitrothiophene-2-carboxaldehyde (10 g, 64 mmol), hydroxylamine hydrochloride (9.4 g, 130 mmol) and sodium hydroxide (4.34 g, 107 mmol) in ethanol/water (150 ml, 2:1) was heated to reflux for 2 hours, then diluted with dichloromethane and washed with water. The organic layer was dried over magnesium sulfate and evaporated to dryness to give 8.8 g of 5-nitro-2-thiophene-carboxaldehyde oxime as a tan solid. 1H NMR (400 MHz, DMSO-d6) δ: 7.54 (1H, d), 8.13 (1H, s), 8.16 (1H, d), 13.14 (1H, s).

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. washwashed with water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-1b980d0a384e46658c2dd869af003b5c
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06528653B2

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