Pyridine → HCID 73852152、化合物

HRID 723229

反応式

HRID 723229 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 73852152HCID 73852152、化合物収率 88%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-43f2ba13baec47cf9648112fe3674629
出典データセット
uspto-grants-2006_11
特許番号
US07138530B2

関連ノート

読み込み中…