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Water → 2-methyl-3-(4-(3-methyl-5-((4-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)-1H-pyrazol-1-yl)propane-1,2-diol

HRID 595305
ノート
印刷プレビュー

反応式

HRID 595305 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([NH:17][C:18]2[N:23]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:21]=[CH:20][N:19]=2)[CH:5]=[C:6]([C:8]2[CH:9]=[N:10][N:11]([CH2:13][C:14]([CH3:16])=[CH2:15])[CH:12]=2)[CH:7]=1.C[N+]1([O-])CC[O:32]CC1.C1COCC1.[OH2:41]>[Os](=O)(=O)(=O)=O>[CH3:15][C:14]([OH:32])([CH2:13][N:11]1[CH:12]=[C:8]([C:6]2[CH:5]=[C:4]([NH:17][C:18]3[N:23]=[C:22]([C:24]([F:26])([F:25])[F:27])[CH:21]=[CH:20][N:19]=3)[CH:3]=[C:2]([CH3:1])[CH:7]=2)[CH:9]=[N:10]1)[CH2:16][OH:41]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 82029Methyl morpholine oxideHCID 118208710N-(3-methyl-5-(1-(2-methylallyl)-1H-pyrazol-4-yl)phenyl)-4-(trifluoromethyl)pyrimidin-2-amine

生成物 1

HCID 1182085542-methyl-3-(4-(3-methyl-5-((4-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)-1H-pyrazol-1-yl)propane-1,2-diol

試薬・触媒・溶媒 1

HCID 30318
Osmium Tetroxide
触媒

実験手順

Osmium tetroxide (290 μl, 0.04 mmol) was added to a flask containing N-(3-methyl-5-(1-(2-methylallyl)-1H-pyrazol-4-yl)phenyl)-4-(trifluoromethyl)pyrimidin-2-amine (56 mg, 0.15 mmol), N-methylmorpholine N-oxide (26.4 mg, 0.225 mmol), THF (1000 μL) and water (500 μL). The reaction mixture was stirred at room temperature for 3.5 hours. Silica was added and the mixture concentrated under reduced pressure. The residue was purified by column chromatography on silica (0-10% MeOH/DCM) and concentrated under reduced pressure. The racemic mixture was purified by chiral SFC (IA column, 40% MeOH with 0.25% DMEA/CO2) to afford 2-methyl-3-(4-(3-methyl-5-((4-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)-1H-pyrazol-1-yl)propane-1,2-diol (Example 21.1, Isomer 1, early eluting): MS ESI calcd. for C19H21F3N5O2 [M+H]+ 408. found 408, 1H NMR δ ppm (DMSO-d6): 10.11 (1H, s), 8.80 (1H, d, J=4.88 Hz), 7.95 (1H, s), 7.81 (1H, s), 7.73 (1H, s), 7.33 (1H, s), 7.24 (1H, d, J=4.88 Hz), 7.05 (1H, s), 4.80 (1H, t, J=5.61 Hz), 4.67 (1H, s), 4.11 (1H, d, J=13.94 Hz), 4.05 (1H, d, J=13.90 Hz), 3.18-3.20 (2H, m), 2.29 (3H, s), 0.95 (3H, s), and 2-methyl-3-(4-(3-methyl-5-((4-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)-1H-pyrazol-1-yl)propane-1,2-diol (Example 21.2, Isomer 2, late eluting): MS ESI calcd. for C19H21F3N5O2 [M+H]+ 408. found 408, 1H NMR δ ppm (DMSO-d6): 10.11 (1H, s), 8.80 (1H, d, J=4.88 Hz), 7.95 (1H, s), 7.81 (1H, s), 7.73 (1H, s), 7.33 (1H, s), 7.24 (1H, d, J=4.88 Hz), 7.05 (1H, s), 4.80 (1H, t, J=5.61 Hz), 4.67 (1H, s), 4.11 (1H, d, J=13.94 Hz), 4.05 (1H, d, J=13.90 Hz), 3.18-3.20 (2H, m), 2.29 (3H, s), 0.95 (3H, s).

後処理

  1. additionSilica was added
  2. concentrationthe mixture concentrated under reduced pressure
  3. customThe residue was purified by column chromatography on silica (0-10% MeOH/DCM)
  4. concentrationconcentrated under reduced pressure
  5. customThe racemic mixture was purified by chiral SFC (IA column, 40% MeOH with 0.25% DMEA/CO2)

出典と根拠

ORDレコード
ord-84d4e28a6a4d4d539478f8a1bd70e474
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…

このページの内容参加物実験手順後処理出典と根拠反応ノート