Diethyl Malonate → HCID 22718000, 화합물

HRID 1582593노트

반응식

HRID 1582593 반응식
[O-]CC.[Na+].[C:5]([O:13][CH2:14][CH3:15])(=[O:12])[CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8].[CH2:16]([O:23][C:24]([NH:26][CH2:27][CH2:28][CH2:29][CH2:30]Br)=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(O)C>[CH2:16]([O:23][C:24]([NH:26][CH2:27][CH2:28][CH2:29][CH2:30][CH:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:5]([O:13][CH2:14][CH3:15])=[O:12])=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

5

반응물 3

HCID 7761Diethyl MalonateHCID 2723922Sodium ethoxideHCID 22714477Benzyl (4-bromobutyl)carbamate

생성물 1

HCID 22718000HCID 22718000, 화합물수율 83%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

An ethanol (130.2 ml) solution of sodium ethoxide (5.83 g) was added with diethyl malonate (13 ml) and stirred at room temperature for 5 minutes. This solution was added with an ethanol (55.8 ml) solution of the 1-benzyloxycarbonylamino-4-bromobutane (4.9 g) obtained in the above step (b), and stirred at 40° C. for 20 hours. The reaction system was concentrated under reduced pressure without any treatment, and the residue was added with saturated aqueous ammonium chloride, and then the organic substances were extracted with ethyl acetate. The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (1.2 kg, hexane:ethyl acetate=2:1) to obtain diethyl 2-(4-benzyloxycarbonylaminobutyl)malonate (5.2 g, 83%).

후처리

  1. customobtained in the above step (b)
  2. stirringstirred at 40° C. for 20 hours
  3. concentrationThe reaction system was concentrated under reduced pressure without any treatment
  4. additionthe residue was added with saturated aqueous ammonium chloride
  5. extractionthe organic substances were extracted with ethyl acetate
  6. concentrationThe organic layer was concentrated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (1.2 kg, hexane:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-e087ff0853d645918bc8eb8fc5a0a963
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737416B2

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