Hydrochloric Acid → 7-Chlorothieno[3,2-b]pyridine-2-carbaldehyde oxime

HRID 500804ノート

反応式

HRID 500804 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([CH:11]=O)[S:10][C:3]=12.[NH2:13][OH:14].Cl>CO.O>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([CH:11]=[N:13][OH:14])[S:10][C:3]=12

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 787HydroxylamineHCID 509888497-Chlorothieno[3,2-b]pyridine-2-carbaldehyde

生成物 1

HCID 1363351767-Chlorothieno[3,2-b]pyridine-2-carbaldehyde oxime収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of aldehyde 14 (scheme 3) in MeOH was added NH2OH×HCl (227 mg, 3.26 mmol) in water (0.5 mL) and the mixture was stirred at room temperature for 0.5 h. The solvents were removed by under reduced pressure and the residue was partitioned between EtOAc and water. The organic phase was dried over anhydrous sodium sulfate, filtered and evaporated to dryness to afford the title compound 125 (458 mg, 85% yield) as a white solid. MS (m/z) 213.1/215.1 (M+H).

後処理

  1. customThe solvents were removed by under reduced pressure
  2. customthe residue was partitioned between EtOAc and water
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-dd877b64733a4894aaf025a0d5b54216
出典データセット
uspto-grants-2010_08
特許番号
US07772247B2

反応ノート

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