1,1,1-Trifluoro-2,4-pentanedione → HCID 178437489, 화합물

HRID 885418노트

반응식

HRID 885418 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

HCID 178437489HCID 178437489, 화합물수율 47%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 8857Ethyl Acetate용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-82b8906f29294553abd2ddc13c046729
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242151B2

반응 노트

불러오는 중…