Potassium Carbonate → ethyl 3-[N,N'-bis(tert-butyloxycarbonyl)hydrazino]-2,5-dioxopyrrolidine-3-carboxylate

HRID 1675932

반응식

HRID 1675932 반응식
[O:1]=[C:2]1[CH:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:5][C:4](=[O:12])[NH:3]1.[N:13]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])=[N:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C>[C:25]([O:24][C:22]([N:13]([C:6]1([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:5][C:4](=[O:12])[NH:3][C:2]1=[O:1])[NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])=[O:23])([CH3:28])([CH3:27])[CH3:26]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 97268Di-tert-butyl azodicarboxylateHCID 23635561Ethyl 2,5-dioxo-3-pyrrolidinecarboxylate

생성물 1

HCID 67342586ethyl 3-[N,N'-bis(tert-butyloxycarbonyl)hydrazino]-2,5-dioxopyrrolidine-3-carboxylate수율 83.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of ethyl 2,5-dioxopyrrolidine-3-carboxylate (2.96 g) in ethyl acetate (25 ml) was added di-tert-butyl azodicarboxylate (4.19 g), followed by potassium carbonate (4.78 g) at room temperature. After this reaction mixture was stirred at room temperature for 15 minutes, the resulting mixture was filtered through a Celite pad and the filtrate was concentrated. The residue was purified by a flash column chromatography (hexane:ethyl acetate=3:1) to give the desired product (5.77 g, 83%) as amorphous.

후처리

  1. filtrationthe resulting mixture was filtered through a Celite pad
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by a flash column chromatography (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-45ae8d89b0024b80b4d4cb53dc70b8f4
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003808B2

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