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1,2-Dichloroethane → N'-Acetyl-4-(Cyclopentylamino)-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide

HRID 490874
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HRID 490874 반응식
[CH:1]1([NH:6][C:7]2[C:12]([C:13]([OH:15])=O)=[CH:11][N:10]=[C:9]3[N:16]([CH2:19][CH3:20])[N:17]=[CH:18][C:8]=23)[CH2:5][CH2:4][CH2:3][CH2:2]1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[C:35]([NH:38][NH2:39])(=[O:37])[CH3:36]>CN(C=O)C>[C:35]([NH:38][NH:39][C:13]([C:12]1[C:7]([NH:6][CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5]2)=[C:8]2[CH:18]=[N:17][N:16]([CH2:19][CH3:20])[C:9]2=[N:10][CH:11]=1)=[O:15])(=[O:37])[CH3:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 14039AcetohydrazideHCID 757711-HydroxybenzotriazoleHCID 576751554-(Cyclopentylamino)-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid

생성물 1

HCID 57675205N'-Acetyl-4-(Cyclopentylamino)-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carbohydrazide수율 54.1%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

Intermediate 3 (0.066 g), EDC (0.06 g) and HOBT (0.035 g) were suspended in DMF (2 ml) and the mixture was stirred for 15 minutes. Acetic hydrazide (0.02 g) was then added and the mixture stirred under nitrogen for 18 h. Solvents were removed by concentration in vacuo and the residue partitioned between DCM and water. The layers were separated and the organic phase was washed with saturated aqueous sodium bicarbonate solution, then concentrated and applied to an SPE cartridge (aminopropyl, 1 g) which was eluted with methanol. Concentration in vacuo afforded Intermediate 4 (0.043 g). LCMS showed MH+=331; TRET=2.38 min.

후처리

  1. stirringthe mixture stirred under nitrogen for 18 h
  2. customSolvents were removed by concentration in vacuo
  3. customthe residue partitioned between DCM and water
  4. customThe layers were separated
  5. washthe organic phase was washed with saturated aqueous sodium bicarbonate solution
  6. concentrationconcentrated
  7. washwas eluted with methanol
  8. concentrationConcentration in vacuo

출처 및 근거

ORD 기록
ord-6918daca97224cb0aa8e8d62b29efc4c
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528148B2

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