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Sodium Pyrosulfite → N-{[6-bromo-2-oxo-4-(trifluoromethyl)-1,2, 3,4-tetrahydroquinazolin-4-yl]methyl}-4-fluorobenzamide

HRID 1878033
ノート
印刷プレビュー

反応式

HRID 1878033 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8](CC1C=CC(OC)=CC=1)[C:7](=[O:21])[NH:6][C:5]2([CH2:26][NH:27][C:28](=[O:36])[C:29]1[CH:34]=[CH:33][C:32]([F:35])=[CH:31][CH:30]=1)[C:22]([F:25])([F:24])[F:23].[N+]([O-])([O-])=O.[NH4+].[Ce].S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+]>C(#N)C.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7](=[O:21])[NH:6][C:5]2([CH2:26][NH:27][C:28](=[O:36])[C:29]1[CH:30]=[CH:31][C:32]([F:35])=[CH:33][CH:34]=1)[C:22]([F:25])([F:23])[F:24]
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 3

HCID 656671Sodium PyrosulfiteHCID 57418452Ammonium cerium-nitrateHCID 68486610N-{[6-bromo-1-(4-methoxybenzyl)-2-oxo-4-(trifluoromethyl)-1,2,3,4-tetrahydroquinazolin-4-yl]methyl}-4-fluorobenzamide

生成物 1

HCID 68488834N-{[6-bromo-2-oxo-4-(trifluoromethyl)-1,2, 3,4-tetrahydroquinazolin-4-yl]methyl}-4-fluorobenzamide

試薬・触媒・溶媒 2

HCID 6342
Acetonitrile
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a stirring solution of N-{[6-bromo-1-(4-methoxybenzyl)-2-oxo-4-(trifluoromethyl)-1,2,3,4-tetrahydroquinazolin-4-yl]methyl}-4-fluorobenzamide (260 mg, 0.46 mmol) in acetonitrile (6 mL), an aqueous solution (1 mL) of cerium ammonium nitrate (755 mg, 1.38 mmol) was added dropwise at room temperature. The reaction solution was stirred at room temperature for 4 hours. Sodium pyrosulfite was added to the reaction solution, and the solution was stirred for 30 minutes, and then diluted with ethyl acetate and the organic layer was separated. The organic layer was washed sequentially with water and saturated brine and then dried over magnesium sulfate. After the drying agent was removed by filtration, the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=2/1), whereby the objective compound (150 mg, 73%) was obtained as a white solid.

後処理

  1. stirringthe solution was stirred for 30 minutes
  2. customthe organic layer was separated
  3. washThe organic layer was washed sequentially with water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customAfter the drying agent was removed by filtration
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=2/1), whereby the objective compound (150 mg, 73%)
  8. customwas obtained as a white solid

出典と根拠

ORDレコード
ord-7601f1823f774a5ea3a1dccd066bb013
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08314094B2

反応ノート

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