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Hydrazine → tert-Butyl 4,6-dihydropyrrolo(3,4-c)pyrazole-5(1H)-carboxylate

HRID 241560
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인쇄 미리보기

반응식

HRID 241560 반응식
[NH2:1]N.C[N:4](/[CH:6]=[C:7]1/[CH2:8][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:10][C:11]/1=O)C>C(O)C>[NH:1]1[C:11]2[CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:8][C:7]=2[CH:6]=[N:4]1
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참가 물질

4

반응물 2

HCID 9321HydrazineHCID 56971730(Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate

생성물 1

HCID 7147072tert-Butyl 4,6-dihydropyrrolo(3,4-c)pyrazole-5(1H)-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of hydrazine (3 mL) and tert-butyl (3Z)-3-[(dimethylamino)methylene]-4-oxopyrrolidine-1-carboxylate (19.22 g) in ethanol (40 mL) was heated at 85° C. in a sealed tube for 4 h. Solvent was removed under reduced pressure, and the residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL). The resulting solid was filtered. The filtrate was concentrated and the resulting solid was triturated again. The combined solids were used in the next step.

후처리

  1. customSolvent was removed under reduced pressure
  2. customthe residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL)
  3. filtrationThe resulting solid was filtered
  4. concentrationThe filtrate was concentrated
  5. customthe resulting solid was triturated again

출처 및 근거

ORD 기록
ord-fd4c7b181d984b04853f1342e9f2316a
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653059B2

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