Aluminum(III) Chloride → 6-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-4-methyl-2(1H)-quinazolinone

HRID 1164798

반응식

HRID 1164798 반응식
[CH3:1][CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][C:4](=[O:12])[NH:3]1.[Cl-].[Al+3].[Cl-].[Cl-].[C:17]([CH2:21][CH:22]([CH3:26])[C:23](Cl)=[O:24])([O:19][CH3:20])=[O:18]>C(=S)=S>[C:17]([CH2:21][CH:22]([CH3:26])[C:23]([C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[NH:5][C:4](=[O:12])[NH:3][CH:2]2[CH3:1])=[O:24])([O:19][CH3:20])=[O:18]

참가 물질

5

반응물 3

HCID 6451240Aluminum(III) ChlorideHCID 123607574-Methyl-3,4-dihydro-1H-quinazolin-2-oneHCID 14403282Methyl 4-chloro-3-methyl-4-oxobutanoate

생성물 1

HCID 146206396-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-4-methyl-2(1H)-quinazolinone

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

3,4-Dihydro-4-methyl-2(1H)-quinazolinone (3.9 g) is added to a stirred suspension of anhydrous aluminum chloride (16.5 g) in carbon disulfide (120 ml) under nitrogen. 3-Carbomethoxy-2-methyl-propionyl chloride (4 g) is added dropwise to the stirred suspension, which is refluxed for about 17 hours and cooled to RT. The liquid phase is decanted and the residue is treated with ice/H2O (150 ml) and extracted with methylene chloride. The organic extract is dried, filtered, and concentrated in vacuo, affording the desired crude product as an oil, which is used in the next step without further purification.

후처리

  1. temperatureis refluxed for about 17 hours
  2. customThe liquid phase is decanted
  3. additionthe residue is treated with ice/H2O (150 ml)
  4. extractionextracted with methylene chloride
  5. extractionThe organic extract
  6. customis dried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2730bdabea554667994afa5299d55c2b
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04906630

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