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

HRID 1607986ノート

反応式

HRID 1607986 の反応式
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][NH:3][C:2]1=[O:11].[Cl-].[Al+3].[Cl-].[Cl-].[C:16]([CH2:20][CH:21]([CH3:25])[C:22](Cl)=[O:23])([O:18][CH3:19])=[O:17]>C(=S)=S>[C:16]([CH2:20][CH:21]([CH3:25])[C:22]([C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[NH:1][C:2](=[O:11])[NH:3][CH2:4]2)=[O:23])([O:18][CH3:19])=[O:17]

参加物

5

反応物 3

HCID 6451240Aluminum(III) ChlorideHCID 123607563,4-Dihydroquinazolin-2(1H)-oneHCID 14403282Methyl 4-chloro-3-methyl-4-oxobutanoate

生成物 1

HCID 146206376-(3-Carbomethoxy-2-methyl-propionyl)-3,4-dihydro-2(1H)-quinazolinone

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

3,4-Dihydro-2(1H)-quinazolinone (3.6 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 tothe stirred suspension, and the reaction mixture refluxed for about 18 hours, cooled to RT and further cooled to 0° C. in an ice bath. The liquid phase is decanted and ice and cold water slowly added to the residue. The aqueous mixture is filtered and the filtered solid suspended and stirred in the anhydrous diethyl ether overnight. The suspension is filtered and the filtered solid used in the next step without further purification.

後処理

  1. temperaturethe reaction mixture refluxed for about 18 hours
  2. temperaturefurther cooled to 0° C. in an ice bath
  3. customThe liquid phase is decanted
  4. additionice and cold water slowly added to the residue
  5. filtrationThe aqueous mixture is filtered
  6. stirringstirred in the anhydrous diethyl ether overnight
  7. filtrationThe suspension is filtered
  8. customthe filtered solid used in the next step without further purification

出典と根拠

ORDレコード
ord-8475f41054b242c1abea36b8d95d2000
出典データセット
uspto-grants-1989_09
特許番号
US04868300

反応ノート

読み込み中…