Water → Ethyl 7-oxoazepane-4-carboxylate

HRID 1620559노트

반응식

HRID 1620559 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 23093698Ethyl 7-oxoazepane-4-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-a6a4d4f17f4649ec96abe580df828ef6
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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