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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
ノート
印刷プレビュー

反応式

HRID 595319 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒
HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-b6f6164b20ba4b069030f6e6f7a54042
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242984B2

反応ノート

読み込み中…

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