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Acetic acid, sodium salt, monohydrate → HCID 178487712, 화합물

HRID 2405675
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HRID 2405675 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[C:4]([N:14]2[CH:18]=[CH:17][C:16]([NH:19][CH:20]([CH3:22])[CH3:21])=[N:15]2)[CH:3]=1.O.C([O-])(=[O:26])C.[Na+]>C(O)(=O)C>[OH:26][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[C:4]([N:14]2[CH:18]=[CH:17][C:16]([NH:19][CH:20]([CH3:22])[CH3:21])=[N:15]2)[CH:3]=1
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4

반응물 2

HCID 23681166Acetic acid, sodium salt, monohydrateHCID 57909998[1-(4-chloro-7-methoxy-quinolin-2-yl)-1H-pyrazol-3-yl]-isopropyl-amine

생성물 1

HCID 178487712HCID 178487712, 화합물수율 19%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
130 °C

실험 절차

A mixture of [1-(4-chloro-7-methoxy-quinolin-2-yl)-1H-pyrazol-3-yl]-isopropyl-amine (0.52 g, 1.6 mmol) and sodium acetate monohydrate (1.0 g) in acetic acid (5 mL) was stirred at 130° C. for 2 d. The mixture was concentrated and then partitioned between ethyl acetate (50 mL) and water (50 mL). The organic layer was concentrated in vacuo. The residue was purified by silica gel column chromatography (ethyl acetate/hexanes), affording [1-(4-hydroxy-7-methoxy-quinolin-2-yl)-1H-pyrazol-3-yl]-isopropyl-amine (0.09 g, 19%). LC/MS=299.1 (M++1).

후처리

  1. concentrationThe mixture was concentrated
  2. custompartitioned between ethyl acetate (50 mL) and water (50 mL)
  3. concentrationThe organic layer was concentrated in vacuo
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-7f9ddaa4f2ad44f1a3df48d4193b4d42
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809266B2

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