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

HRID 606479ノート

反応式

HRID 606479 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-f7a7079f6dda402e8eaed25a632e2472
出典データセット
uspto-grants-2011_03
特許番号
US07915267B2

反応ノート

読み込み中…