Pyridine → HCID 73852152, 화합물

HRID 723229

반응식

HRID 723229 반응식
Cl.[NH2:2][OH:3].[Br:4][C:5]1[CH:6]=[C:7]([CH:13]=O)[S:8][C:9]=1[N+:10]([O-:12])=[O:11].N1C=CC=CC=1>CCO>[Br:4][C:5]1[CH:6]=[C:7]([CH:13]=[N:2][OH:3])[S:8][C:9]=1[N+:10]([O-:12])=[O:11]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 218862814-Bromo-5-nitrothiophene-2-carbaldehyde

생성물 1

HCID 73852152HCID 73852152, 화합물수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Hydroxylamine hydrochloride (85 g, 1.2 mol) was added to a solution of 4-bromo-5-nitro-thiophene-2-carbaldehyde (234 mg, 0.529 mmol, Example 286: step a) in EtOH (7.5 mL, 200 proof—anhydrous):pyridine (100 mL, anhydrous) at rt over 5 min. The reaction mixture was heated to reflux overnight, then cooled to rt. The solvents were removed in vacuo resulting in a solid residue that was washed with water and filtered. The solid was dried overnight under high vacuum to afford the title compound as a yellow solid (225 g, 88%). The solid was used for the next step without further characterization.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux overnight
  3. customThe solvents were removed in vacuo
  4. customresulting in a solid residue that
  5. washwas washed with water
  6. filtrationfiltered
  7. customThe solid was dried overnight under high vacuum

출처 및 근거

ORD 기록
ord-43f2ba13baec47cf9648112fe3674629
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138530B2

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