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

HRID 1164798ノート

反応式

HRID 1164798 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2730bdabea554667994afa5299d55c2b
出典データセット
uspto-grants-1990_03
特許番号
US04906630

反応ノート

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