Sodium Carbonate → HCID 86745294, 화합물

HRID 1461039노트

반응식

HRID 1461039 반응식
[CH2:1]([N:8]1[CH2:12][C:11](=O)[CH:10]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:20][OH:21].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.O>[CH2:1]([N:8]1[CH2:12][C:11](=[N:20][OH:21])[CH:10]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 274831Ethyl 1-benzyl-4-oxopyrrolidine-3-carboxylateHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 86745294HCID 86745294, 화합물수율 60.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 24.7 g (0.1 mole) of 1-benzyl-3-ethoxycarbonyl-4-pyrrolidone in 135 ml of ethanol was added dropwise at room temperature to a solution of 34.7 g (0.5 mole) of hydroxylamine hydrochloride dissolved in 135 ml of water, and then 28.1 g (0.265 mole) of sodium carbonate were added to the mixture. The mixture was then stirred at room temperature for 6.5 hours, after which it was extracted with 300 ml of chloroform. The chloroform extract was washed with water and dried over anhydrous sodium sulfate. It was then concentrated by evaporation under reduced pressure. The residue was purified by column chromatography through silica gel using a 2:1 by volume mixture of toluene and ethyl acetate as the eluent, to afford 15.8 g of 1-benzyl-3-ethoxycarbonyl-4-hydroxyiminopyrrolidine as a brown oil.

후처리

  1. extractionafter which it was extracted with 300 ml of chloroform
  2. extractionThe chloroform extract
  3. washwas washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationIt was then concentrated by evaporation under reduced pressure
  6. customThe residue was purified by column chromatography through silica gel using a 2:1
  7. additionby volume mixture of toluene and ethyl acetate as the eluent

출처 및 근거

ORD 기록
ord-c1f1957dd6aa4f70b12777a629420d4d
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05073556

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