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HCID 11845250, 화합물 → HCID 11847134, 화합물

HRID 1158892
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HRID 1158892 반응식
[N+:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]3[N:18]=[C:19]([CH2:21][OH:22])[CH:20]=[C:14]3[CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]>O=[Mn]=O.C(Cl)(Cl)Cl.CO>[N+:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][O:9][C:10]([N:12]2[CH2:17][CH2:16][N:15]3[N:18]=[C:19]([CH:21]=[O:22])[CH:20]=[C:14]3[CH2:13]2)=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 11845250HCID 11845250, 화합물

생성물 1

HCID 11847134HCID 11847134, 화합물

시약·촉매·용매 2

HCID 14801Manganese dioxide촉매HCID 21584188Chloroform methanol용매

실험 절차

MnO2 (activated) (84.2 g) was added to the CHCl3-MeOH (95:5, 253 mL) solution of 2-hydroxymethyl-6,7-dihydro-4H-pyrazolo[1,5-a]pyrazine-5-carboxylic acid 4-nitrobenzyl ester (8.42 g), and the mixture was refluxed for 1 h under a nitrogen atmosphere. The reaction mixture was filtered through a pad of Celite. Silica-gel (20 g) was added to the filtrate and the solvent was removed under reduced pressure to give the silica-gel coating with crude reactant. The above silica-gel was adsorbed to silica-gel column chromatography and the column was eluted with CHCl3-MeOH (49/1 to 19/1). The titled compound was obtained as yellow crystals (2.82 g, 34%).

후처리

  1. temperaturethe mixture was refluxed for 1 h under a nitrogen atmosphere
  2. filtrationThe reaction mixture was filtered through a pad of Celite
  3. additionSilica-gel (20 g) was added to the filtrate
  4. customthe solvent was removed under reduced pressure
  5. customto give the silica-gel coating with crude reactant
  6. washthe column was eluted with CHCl3-MeOH (49/1 to 19/1)

출처 및 근거

ORD 기록
ord-e7ee7bd354054811aa814a0b432c16b0
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812014B2

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