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Ammonium Hydroxide → racemic 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzamide

HRID 595319
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HRID 595319 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([C:15]2[CH:16]=[N:17][N:18]([CH:20]([C:22]3[CH:30]=[CH:29][C:25]([C:26](O)=[O:27])=[CH:24][CH:23]=3)[CH3:21])[CH:19]=2)[CH:5]=[C:6]([NH:8][C:9]2[N:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:7]=1.[OH-].[NH4+:32]>C1COCC1.CN(C=O)C.C(OCC)(=O)C.O>[CH3:1][C:2]1[CH:3]=[C:4]([C:15]2[CH:16]=[N:17][N:18]([CH:20]([C:22]3[CH:30]=[CH:29][C:25]([C:26]([NH2:32])=[O:27])=[CH:24][CH:23]=3)[CH3:21])[CH:19]=2)[CH:5]=[C:6]([NH:8][C:9]2[N:10]=[CH:11][CH:12]=[CH:13][N:14]=2)[CH:7]=1
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참가 물질

7

반응물 2

HCID 14923Ammonium HydroxideHCID 1182088364-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzoic acid

생성물 1

HCID 118208806racemic 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzamide

시약·촉매·용매 4

HCID 962Water용매HCID 6228Dimethylformamide용매
HCID 8028
Tetrahydrofuran
용매
HCID 8857Ethyl Acetate용매

실험 절차

2-(1H-Benzo[d][1,2,3]triazol-1-yl)-1,1,3,3-tetramethylisouronium tetrafluoroborate (101 mg, 0.315 mmol) was added to a solution of 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzoic acid (105 mg, 0.263 mmol) in THF (5.0 mL) and DMF (1.0 mL). Ammonium hydroxide (0.15 mL, 1.05 mmol) was then added and the reaction mixture was stirred at ambient temperature for 1 hour. The reaction mixture was diluted with ethyl acetate (100 mL) and water (10 mL). The organic layer was separated and washed with water (2×10 mL) followed by brine (10 mL). The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to afford the crude product residue. The crude product residue was purified by column chromatography on silica (0-100% [5% methanol in ethyl acetate]/hexanes) to afford racemic 4-(1-(4-(3-methyl-5-(pyrimidin-2-ylamino)phenyl)-1H-pyrazol-1-yl)ethyl)benzamide. MS ESI calcd. for C23H23N6O [M+H]+ 399. found 399. 1H NMR (500 MHz, DMSO-d6) δ 9.46 (s, 1H), 8.46 (d, J=5.0 Hz, 2H), 8.22 (s, 1H), 7.92 (s, 1H), 7.82 (s, 1H), 7.79 (d, J=6.5 Hz, 2H), 7.71 (s, 1H), 7.41 (s, 1H), 7.36-7.26 (m, 3H), 7.00 (s, 1H), 6.80 (t, J=5.0 Hz, 1H), 5.70-5.64 (m, 1H), 2.27 (s, 3H), 1.83 (d, J=7.0 Hz, 3H).

후처리

  1. customThe organic layer was separated
  2. washwashed with water (2×10 mL)
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto afford the crude product residue
  7. customThe crude product residue was purified by column chromatography on silica (0-100% [5% methanol in ethyl acetate]/hexanes)

출처 및 근거

ORD 기록
ord-b6f6164b20ba4b069030f6e6f7a54042
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242984B2

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