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

HRID 490874
ノート
印刷プレビュー

反応式

HRID 490874 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6918daca97224cb0aa8e8d62b29efc4c
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07528148B2

反応ノート

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