2(3H)-Benzoxazolone → 6-(3-Chloropropanoyl)-1,3-benzoxazol-2(3H)-one

HRID 654433노트

반응식

HRID 654433 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH:5]1[CH:6]=[CH:7][C:8]2[O:14][C:12](=[O:13])[NH:11][C:9]=2[CH:10]=1.[Cl:15][CH2:16][CH2:17][C:18](Cl)=[O:19]>CN(C)C=O>[Cl:15][CH2:16][CH2:17][C:18]([C:6]1[CH:5]=[CH:10][C:9]2[NH:11][C:12](=[O:13])[O:14][C:8]=2[CH:7]=1)=[O:19]

참가 물질

5

반응물 3

HCID 60432(3H)-BenzoxazoloneHCID 693643-Chloropropionyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 117908766-(3-Chloropropanoyl)-1,3-benzoxazol-2(3H)-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

56.1 g (0.42 mole) of aluminum chloride are weighed into a ground-necked flask, 10 cm3 of dimethylformamide are then added using a dropping funnel and the mixture is left stirring until it becomes homogeneous. 8.1 g (0.06 mole) of benzoxazolinone are then added and the mixture is left stirring for 10 minutes before adding 7 cm3 (0.072 mole) of 3-chloropropionic acid chloride. This mixture is maintained in an oil bath at 80°-85° C. for approximately 2 hours 30 minutes. After cooling, the reaction mixture is poured into ice-cold water. The precipitate is drained and washed with water to neutrality. The product is recrystallized in ethanol.

후처리

  1. waitthe mixture is left
  2. waitthe mixture is left
  3. stirringstirring for 10 minutes
  4. temperatureThis mixture is maintained in an oil bath at 80°-85° C. for approximately 2 hours 30 minutes
  5. temperatureAfter cooling
  6. additionthe reaction mixture is poured into ice-cold water
  7. washwashed with water to neutrality
  8. customThe product is recrystallized in ethanol

출처 및 근거

ORD 기록
ord-115e79cdb56f45cb9e47650fe4e039df
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05132305

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