Aluminum(III) Chloride → 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one

HRID 469296

반응식

HRID 469296 반응식
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8](Cl)=[O:9])[CH:3]=1.[Cl-].[Cl-].[Cl-].[Al+3].[CH3:15][C:16]1[C:21]2[NH:22][C:23](=[O:25])[O:24][C:20]=2[CH:19]=[CH:18][CH:17]=1>>[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8]([C:18]2[CH:17]=[C:16]([CH3:15])[C:21]3[NH:22][C:23](=[O:25])[O:24][C:20]=3[CH:19]=2)=[O:9])[CH:3]=1

참가 물질

4

반응물 3

HCID 6451240Aluminum(III) ChlorideHCID 127093364-Methyl-3H-benzooxazol-2-oneHCID 184220986-Chloropyrimidine-4-carbonyl chloride

생성물 1

HCID 581812066-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one

반응 조건

온도
130 °C

실험 절차

A well stirred mixture of 2.34 g (13.2 mmol) 6-chloropyrimidine-4-carboxylic acid chloride, 8.00 g (60.0 mmol) aluminium trichloride and 1.79 g (12.0 mmol) 4-methyl-3H-benzoxazol-2-one was heated to 130° C. for 1.5 h. After cooling to RT the mixture was decomposed with ice water, then extracted with ethyl acetate, the organic phase was dried on sodium sulphate and evaporated down i. vac. The crude product left as a solid was triturated with diethyl ether, suction filtered and dried in the air.

후처리

  1. temperatureAfter cooling to RT the mixture
  2. extractionextracted with ethyl acetate
  3. customthe organic phase was dried on sodium sulphate
  4. customevaporated down i
  5. waitThe crude product left as a solid
  6. customwas triturated with diethyl ether, suction
  7. filtrationfiltered
  8. customdried in the air

출처 및 근거

ORD 기록
ord-c961173ac0b74a0d908d78f18e71632f
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629137B2

연결된 노트

불러오는 중…