Carbon Disulfide → 6-(3-Carbomethoxy-3-methyl-propionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

HRID 2231931ノート

反応式

HRID 2231931 の反応式
[CH3:1][N:2]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:4][C:3]1=[O:12].[Cl-].[Al+3].[Cl-].[Cl-].[C:17]([CH2:21][CH:22](C)[C:23](Cl)=[O:24])([O:19][CH3:20])=[O:18].[C:27](=S)=S>>[C:17]([CH:21]([CH3:27])[CH2:22][C:23]([C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[NH:4][C:3](=[O:12])[N:2]([CH3:1])[CH2:11]2)=[O:24])([O:19][CH3:20])=[O:18]

参加物

5

反応物 4

HCID 6348Carbon DisulfideHCID 38465583,4-Dihydro-3-methyl-2(1H)-quinazolinoneHCID 6451240Aluminum(III) ChlorideHCID 14403282Methyl 4-chloro-3-methyl-4-oxobutanoate

生成物 1

HCID 198633366-(3-Carbomethoxy-3-methyl-propionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

実験手順

3,4-Dihydro-3-methyl-2(1H)-quinazolinone (2.5 g) is added to a stirred suspension of anhydrous aluminum chloride (10.5 g) in carbon disulfide (120 ml) under nitrogen. 3-Carbomethoxy-2-methyl-propionyl chloride (2.5 g) is added dropwise to the stirred suspension, which is refluxed for about 18 hours and cooled to RT. The liquid phase is decanted and the residue treated with H2O (120 ml) and extracted with methylene chloride. The organic extract is dried, filtered and concentrated in vacuo, affording the desired product as a solid, which is used in the next step without further purification.

後処理

  1. temperatureis refluxed for about 18 hours
  2. customThe liquid phase is decanted
  3. additionthe residue treated with H2O (120 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-bbfdfbeec3ec402db425c8e50135c687
出典データセット
uspto-grants-1988_11
特許番号
US04785101

反応ノート

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