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Acetamide → HCID 24905232, 화합물

HRID 731860
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HRID 731860 반응식
Cl[C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:12]3[C:20]4[C:15](=[N:16][CH:17]=[N:18][C:19]=4[NH2:21])[N:14]([CH:22]([CH3:24])[CH3:23])[N:13]=3)[CH:8]=2)[N:3]=1.C([NH2:28])(=O)C.C([O-])([O-])=O.[K+].[K+]>>[NH2:21][C:19]1[N:18]=[CH:17][N:16]=[C:15]2[N:14]([CH:22]([CH3:23])[CH3:24])[N:13]=[C:12]([C:7]3[CH:8]=[C:9]4[C:4](=[CH:5][CH:6]=3)[N:3]=[C:2]([NH2:28])[CH:11]=[CH:10]4)[C:20]=12
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참가 물질

4

반응물 3

HCID 178AcetamideHCID 11430Potassium CarbonateHCID 24905216HCID 24905216, 화합물

생성물 1

HCID 24905232HCID 24905232, 화합물수율 46%

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온도
200 °C

실험 절차

3-(2-chloroquinolin-6-yl)-1-isopropyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine (BA130, 50 mg, 0.15 mmol), acetamide (174 mg, 3.0 mmol) and K2CO3 (104 mg, 0.75 mmol) were combined and heated to 200° C. under an argon atmosphere for one hour. Reaction was cooled, then extracted with H2O and CH2Cl2. Organic phases were combined, concentrated in vacuo and purified by RP-HPLC (MeCN:H2O:0.1% TFA) to yield BA146 (22 mg, 46% yield). ESI-MS (M+H)+ m/z calcd 320.2, found 320.4.

후처리

  1. customReaction
  2. temperaturewas cooled
  3. extractionextracted with H2O and CH2Cl2
  4. concentrationconcentrated in vacuo
  5. custompurified by RP-HPLC (MeCN:H2O:0.1% TFA)

출처 및 근거

ORD 기록
ord-bdd0fe0ea8454b9e872b1229ded57597
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585868B2

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