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Ethyl Acetate → 2-(5-chloro-2-(1-isopropyl-3-methyl-1H-pyrazol-5-ylamino)pyridin-4-ylamino)benzoic acid

HRID 62494
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HRID 62494 반응식
[Cl:1][C:2]1[C:3]([NH:18][C:19]2C=[CH:25][CH:24]=[CH:23][C:20]=2C#N)=[CH:4][C:5]([NH:8][C:9]2[N:13]([CH:14]([CH3:16])[CH3:15])[N:12]=[C:11]([CH3:17])[CH:10]=2)=[N:6][CH:7]=1.[OH-].[Na+].[C:29]([O:32]CC)(=[O:31])[CH3:30]>O1CCOCC1>[Cl:1][C:2]1[C:3]([NH:18][C:19]2[CH:20]=[CH:23][CH:24]=[CH:25][C:30]=2[C:29]([OH:32])=[O:31])=[CH:4][C:5]([NH:8][C:9]2[N:13]([CH:14]([CH3:15])[CH3:16])[N:12]=[C:11]([CH3:17])[CH:10]=2)=[N:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 593144562-(5-chloro-2-(1-isopropyl-3-methyl-1H-pyrazol-5-ylamino)pyridin-4-ylamino)benzonitrile

생성물 1

HCID 593144592-(5-chloro-2-(1-isopropyl-3-methyl-1H-pyrazol-5-ylamino)pyridin-4-ylamino)benzoic acid수율 76%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2-[(5-Chloro-2-{[3-methyl-1-(1-methylethyl)-1H-pyrazol-5-yl]amino}-4-pyridinyl)amino]benzonitrile (80 g, 218 mmol) was dissolved in 1,4-dioxane (1.5 L) and 1 M NaOH (1500 mL, 1500 mmol) was added. The suspension was refluxed overnight. After cooling to RT, ethyl acetate (1 L) was added and layers were separated. The water layer was washed with 1 L of ethyl acetate. Both organic layers were combined and backwashed with 0.1 M NaOH (1 L) until no product was observed in organic. The organics were then discarded. Combined aqueous were then washed with 1 L of ethyl acetate. The water layer was then acidified with acetic acid (very slowly to ph˜7). The solid was filtered and 2-[(5-chloro-2-{[3-methyl-1-(1-methylethyl)-1H-pyrazol-5-yl]amino}-4-pyridinyl)amino]benzoic acid (67 g, 165 mmol, 76% yield) was isolated as a yellow solid. 1H NMR (400 MHz, DMSO-d6) ppm 1.28 (d, J=6.57 Hz, 6 H) 2.11 (s, 3 H) 4.41 (quin, J=6.57 Hz, 1 H) 5.96 (s, 1 H) 6.83 (s, 1 H) 7.09 (ddd, J=8.02, 5.12, 3.03 Hz, 1 H) 7.40 (1 H) 7.52-7.61 (m, 2 H) 7.91-8.16 (m, 2 H) 8.55 (s, 1 H) 10.17 (brs, 1 H) 13.64 (brs, 1 H); HPLC Rt=2.35 min, MS (ESI): [M+H]+=386.1.

후처리

  1. temperatureThe suspension was refluxed overnight
  2. customlayers were separated
  3. washThe water layer was washed with 1 L of ethyl acetate
  4. washCombined aqueous were then washed with 1 L of ethyl acetate
  5. filtrationThe solid was filtered

출처 및 근거

ORD 기록
ord-c6a08fe10e4c49eeaabc791aa39f60d9
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09446034B2

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