Potassium Carbonate → N-benzoyl-N'-t-butyl-N'-(ethoxycarbonyl)methylhydrazine

HRID 21663

반응식

HRID 21663 반응식
[C:1]([NH:5][NH:6][C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[C:21]([O:24][CH2:25][CH2:26]Br)(=[O:23])[CH3:22]>CN(C)C=O.O.CCOCC>[C:7]([NH:6][N:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH2:22][C:21]([O:24][CH2:25][CH3:26])=[O:23])(=[O:14])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 299436N'-tert-butylbenzohydrazide

생성물 1

HCID 15452013N-benzoyl-N'-t-butyl-N'-(ethoxycarbonyl)methylhydrazine수율 9.4%

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

N'-t-butyl-N-benzoylhydrazine (2.0 g), powdered potassium carbonate (5 g) and bromoethyl acetate (1.6 g) were stirred in dimethylformamide (20 ml) at 60° C. for 14 hours. The reaction mixture was diluted with water and ether, and the organic layer was separated. The organic layer was washed several times with water, dried over magnesium sulfate and rotavapped to afford an oil. Chromatographic purification gave the pure oil product (0.25 g).

후처리

  1. customthe organic layer was separated
  2. washThe organic layer was washed several times with water
  3. dry with materialdried over magnesium sulfate
  4. customto afford an oil
  5. customChromatographic purification

출처 및 근거

ORD 기록
ord-037e49102d464965acd586fc010b4458
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424333

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