Triethylamine → Ethyl ((2-(aminocarbonyl)-4-fluorophenyl)amino)(oxo)acetate

HRID 606479노트

반응식

HRID 606479 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].C(N(CC)CC)C.Cl[C:20](=[O:26])[C:21]([O:23][CH2:24][CH3:25])=[O:22]>C1COCC1.C(OCC)(=O)C>[NH2:6][C:4]([C:3]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:2]=1[NH:1][C:20](=[O:26])[C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:5]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 102410032-Amino-5-fluorobenzamide

생성물 1

HCID 66768981Ethyl ((2-(aminocarbonyl)-4-fluorophenyl)amino)(oxo)acetate수율 87.1%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-amino-5-fluorobenzamide (2.00 g, 13.0 mmol) and triethylamine (1.45 g, 14.3 mmol) in THF (40 mL) was added dropwise ethyl chloroglyoxylate (1.95 g, 14.3 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was washed with ethanol to give ethyl ((2-(aminocarbonyl)-4-fluorophenyl)amino)(oxo)acetate as a white powder (2.88 g, 87%).

후처리

  1. temperaturecooling
  2. washwashed with water and saturated brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. washThe residue was washed with ethanol

출처 및 근거

ORD 기록
ord-f7a7079f6dda402e8eaed25a632e2472
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915267B2

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