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1-Propanol → HCID 66958580、化合物

HRID 2283772
ノート
印刷プレビュー

反応式

HRID 2283772 の反応式
[CH2:1]([N:8]1[C:12]([CH3:13])=[C:11](Br)[C:10]([C:15]#[N:16])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:17][C:18]([CH3:32])([CH3:31])[C:19]([NH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1B(O)O)=[O:20].C(O)CC.C(=O)([O-])[O-].[Na+].[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(OC)(C)(C)C.O>[CH2:1]([N:8]1[C:12]([CH3:13])=[C:11]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[NH:21][C:19](=[O:20])[C:18]([CH3:31])([CH3:17])[CH3:32])[C:10]([C:15]#[N:16])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 10311-PropanolHCID 10340Sodium CarbonateHCID 41935022-(Pivalamido)phenylboronic AcidHCID 669586391-Benzyl-4-bromo-5-methyl-1H-pyrazole-3-carbonitrile

生成物 1

HCID 66958580HCID 66958580、化合物収率 59.1%

試薬・触媒・溶媒 4

HCID 11776
Triphenylphosphine
触媒
HCID 167845palladium(II) acetate触媒
HCID 962Water溶媒
HCID 15413tert-Butyl methyl ether溶媒

実験手順

1-Benzyl-4-bromo-5-methyl-1H-pyrazole-3-carbonitrile (3.00 g, 10.9 mmol) was treated with triphenylphosphine (85 mg, 0.32 mmol), 2-[(2,2-dimethylpropanoyl)amino]phenylboronic acid (prepared as described in Part G of Example 23, 2.15 g, 16.3 mmol), 1-propanol (22 mL), palladium (II) acetate (24 mg, 0.11 mmol), aqueous sodium carbonate (6.5 mL of 2 M, 13 mmol), and water (4.4 mL) according to the general procedure described in Example 34. The reaction time was approximately 16 hours and no additional reagents were added. The reaction was allowed to cool to ambient temperature and methyl tert-butyl ether (25 mL) was added. After the mixture was stirred for about 10 minutes, the layers were separated. The organic layer was dried over magnesium sulfate, filtered, and concentrated to yield a brown oil. The crude product was purified by chromatography on a HORIZON HPFC system (silica gel, gradient elution 1-30% ethyl acetate in hexanes). The appropriate fractions were combined, dried over magnesium sulfate, filtered, and concentrated to yield 2.40 g of N-[2-(1-benzyl-3-cyano-5-methyl-1H-pyrazol-4-yl)phenyl]-2,2-dimethylpropanamide as an oil that solidified upon standing at ambient temperature.

後処理

  1. additionno additional reagents were added
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto yield a brown oil
  7. customThe crude product was purified by chromatography on a HORIZON HPFC system (silica gel, gradient elution 1-30% ethyl acetate in hexanes)
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-63e9d0e84f8d4b19851fc2f1bbb86499
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09145410B2

反応ノート

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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