Ammonium Chloride → 4-Methyl-4-phenyl-3,4-dihydro-1H-quinazolin-2-one

HRID 1497734ノート

反応式

HRID 1497734 の反応式
[C:1]1([C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[NH:10][C:9](=[O:17])[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:18][Mg]Br.[NH4+].[Cl-]>C1COCC1>[CH3:18][C:7]1([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:10][C:9](=[O:17])[NH:8]1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 634302(1H)-Quinazolinone, 4-phenyl-HCID 178418573HCID 178418573、化合物

生成物 1

HCID 1176010134-Methyl-4-phenyl-3,4-dihydro-1H-quinazolin-2-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-Phenyl-1H-quinazolin-2-one (5.0 g, 4.5 mmol) in THF (50 ml) is added methylmagnesium bromide (15.0 ml) dropwise at −78° C. under nitrogen. The mixture is stirred overnight at room temperature. The mixture is poured into an aqueous solution of NH4Cl and then extracted with EtOAc. The organic phase is washed with brine, dried over Na2SO4, filtered and evaporated under reduced pressure. The residue is purified on silica gel to give product as a white solid.

後処理

  1. extractionextracted with EtOAc
  2. washThe organic phase is washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue is purified on silica gel
  7. customto give product as a white solid

出典と根拠

ORDレコード
ord-2394edaa774548dda0671e282f6907e3
出典データセット
uspto-grants-2015_12
特許番号
US09199988B2

反応ノート

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