Ethanol → HCID 135482330, 화합물

HRID 1692729

반응식

HRID 1692729 반응식
[NH2:1][C:2]1[N:6]([CH:7]2[CH2:11][CH2:10][CH2:9][CH2:8]2)[N:5]=[CH:4][C:3]=1[C:12]([NH2:14])=[O:13].[Cl:15][C:16]1[CH:17]=[C:18]([CH2:22][C:23](OCC)=O)[CH:19]=[CH:20][CH:21]=1.C(O)C.[H-].[Na+]>O>[Cl:15][C:16]1[CH:17]=[C:18]([CH:19]=[CH:20][CH:21]=1)[CH2:22][C:23]1[NH:14][C:12](=[O:13])[C:3]2[CH:4]=[N:5][N:6]([CH:7]3[CH2:11][CH2:10][CH2:9][CH2:8]3)[C:2]=2[N:1]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 24758Sodium hydrideHCID 8063366Ethyl 2-(3-chlorophenyl)acetateHCID 117011915-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide

생성물 1

HCID 135482330HCID 135482330, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Under argon, 180 mg (0.91 mmol) of 5-amino-1-cyclopentyl-1H-pyrazole-4-carboxamide and 575 mg (2.72 mmol; 3 equiv.) of ethyl (3-chlorophenyl)acetate are introduced into 3.5 ml of absolute ethanol. At 0° C., 127 mg of sodium hydride (60% dispersion in mineral oil; 3.18 mmol; 3.5 equiv.) are slowly added in a countercurrent of argon. The resulting mixture is slowly warmed and stirred under reflux for 18 h. The mixture is worked up by adding 50 ml of water and extracted several times with ethyl acetate. The combined organic phases are dried over sodium sulfate and concentrated in vacuo. The crude product is purified by preparative HPLC.

후처리

  1. temperatureThe resulting mixture is slowly warmed
  2. temperatureunder reflux for 18 h
  3. extractionextracted several times with ethyl acetate
  4. dry with materialThe combined organic phases are dried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe crude product is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-31b26db9e03744e59abc79ad8d68d153
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158633B2

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