1,1,1-Trifluoro-2,4-pentanedione → HCID 178437489、化合物

HRID 885418ノート

反応式

HRID 885418 の反応式
Cl.[C:2](=[NH:8])(OCC)[CH2:3][CH3:4].Cl.[NH2:10][CH2:11][C:12]#[N:13].[F:14][C:15]([F:23])([F:22])[C:16](=O)[CH2:17][C:18](=O)[CH3:19].C(N(C(C)C)CC)(C)C>ClCCCl.C(OCC)(=O)C>[CH2:3]([C:2]1[NH:8][C:11]2=[N:10][C:18]([CH3:19])=[CH:17][C:16]([C:15]([F:23])([F:22])[F:14])=[C:12]2[N:13]=1)[CH3:4]

参加物

7

反応物 4

HCID 739431,1,1-Trifluoro-2,4-pentanedioneHCID 81531DiisopropylethylamineHCID 11491918Aminoacetonitrile hydrochlorideHCID 13000588Ethyl propanecarboximidate hydrochloride

生成物 1

HCID 178437489HCID 178437489、化合物収率 47%

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Ethyl propionimidate hydrochloride (1.37 g, 10.0 mmol), aminoacetonitrile hydrochloride (0.93 g, 10.0 mmol), 1,1,1-trifluoro-2,4-pentanedione (3.64 mL, 30.0 mmol) and diisopropylethylamine (5.23 mL, 30.0 mmol) were stirred in 1,2-dichloroethane (50 mL) under reflux for 4 hr. Ethyl acetate was added to the mixture, and the mixture was washed with water and brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=30/70) to give the title compound (1.07 g, 47%).

後処理

  1. temperatureunder reflux for 4 hr
  2. washthe mixture was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=30/70)

出典と根拠

ORDレコード
ord-82b8906f29294553abd2ddc13c046729
出典データセット
uspto-grants-2012_08
特許番号
US08242151B2

反応ノート

読み込み中…