Hydroxyamine hydrochloride → 3-Fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde oxime

HRID 1527468ノート

反応式

HRID 1527468 の反応式
[F:1][C:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=O.Cl.[NH2:15][OH:16].C([O-])(=O)C.[NH4+]>CO.O>[F:1][C:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=[N:15][OH:16]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517165Ammonium AcetateHCID 866738643-Fluoro-2-(trifluoromethyl)pyridine-4-carbaldehyde

生成物 1

HCID 1363523253-Fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde oxime

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 3-fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde (0.495 g, 2.05 mmol) in MeOH (17.6 mL) and water (2.9 mL) were added hydroxylamine hydrochloride (0.214 g, 3.08 mmol) and ammonium acetate (0.474 g, 6.15 mmol), and the resulting mixture was stirred at RT overnight. Volatile were removed in vacuo, and the residue was suspended in CH2Cl2/MeOH 9:1. The precipitate was filtered off, washed with CH2Cl2 and dried to afford the title compound as a white solid. MS (LC/MS): 209.0 [M+H]+; tR (HPLC conditions c): 4.28 min.

後処理

  1. customVolatile were removed in vacuo
  2. filtrationThe precipitate was filtered off
  3. washwashed with CH2Cl2
  4. customdried

出典と根拠

ORDレコード
ord-423f296eef0f41c09ce34e77d16bcefb
出典データセット
uspto-grants-2015_07
特許番号
US09085555B2

反応ノート

読み込み中…