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

HRID 1497734

반응식

HRID 1497734 반응식
[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

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 634302(1H)-Quinazolinone, 4-phenyl-HCID 178418573HCID 178418573, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2394edaa774548dda0671e282f6907e3
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09199988B2

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