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

HRID 1607986

반응식

HRID 1607986 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8475f41054b242c1abea36b8d95d2000
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04868300

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