Water → Ethyl 7-oxoazepane-4-carboxylate

HRID 1620559ノート

反応式

HRID 1620559 の反応式
ClC1N=C(Cl)N=C(Cl)N=1.O[N:11]=[C:12]1[CH2:17][CH2:16][CH:15]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:14][CH2:13]1.[OH2:23]>CN(C=O)C>[O:23]=[C:12]1[NH:11][CH2:17][CH2:16][CH:15]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 962WaterHCID 7954Cyanuric chlorideHCID 11593553Cyclohexanecarboxylic acid, 4-(hydroxyimino)-, ethyl ester

生成物 1

HCID 23093698Ethyl 7-oxoazepane-4-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 2,4,6-trichloro-1,3,5-triazine (21.7 g) in DMF (25 mL) was added dropwise ethyl 4-(hydroxyimino)cyclohexanecarboxylate (27.2 g) in DMF (220 mL) over 30 min. The mixture was stirred at room temperature overnight, poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give ethyl 7-oxoazepane-4-carboxylate (2.40 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-a6a4d4f17f4649ec96abe580df828ef6
出典データセット
uspto-grants-2014_07
特許番号
US08772277B2

反応ノート

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