Triethylamine → 2-[1-(5-Bromo-3-Thienyl)-2-Nitroethyl]-4-(p-Chlorophenyl)-2-(Trifluoromethyl)-3-Oxazolin-5-One

HRID 374529노트

반응식

HRID 374529 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:19](=[O:20])[O:18][CH:17]([C:21]([F:24])([F:23])[F:22])[N:16]=2)=[CH:11][CH:10]=1.[Br:25][C:26]1[S:27][CH:28]=[C:29]([CH:31]=[CH:32][N+:33]([O-:35])=[O:34])[CH:30]=1>C1(C)C=CC=CC=1.Cl.CCOCC>[Br:25][C:26]1[S:27][CH:28]=[C:29]([CH:31]([C:17]2([C:21]([F:22])([F:24])[F:23])[N:16]=[C:15]([C:12]3[CH:11]=[CH:10][C:9]([Cl:8])=[CH:14][CH:13]=3)[C:19](=[O:20])[O:18]2)[CH2:32][N+:33]([O-:35])=[O:34])[CH:30]=1

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 110652915(2H)-Oxazolone, 4-(4-chlorophenyl)-2-(trifluoromethyl)-HCID 54097949HCID 54097949, 화합물

생성물 1

HCID 194192982-[1-(5-Bromo-3-Thienyl)-2-Nitroethyl]-4-(p-Chlorophenyl)-2-(Trifluoromethyl)-3-Oxazolin-5-One

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 1140Toluene용매2회HCID 3283Diethyl Ether용매

실험 절차

A solution of triethylamine (0.30 g, 3 mmol) in toluene is added to a solution of 4-(p-chlorophenyl)-2-(trifluoromethyl)-3-oxazolin-5-one (10.0 g, 38 mmol) and 2-bromo-4-(2-nitrovinyl)thiophene (8.98 g, 32 mmol) in toluene at 0° C. The reaction mixture is warmed to room temperature and diluted with dilute hydrochloric acid and ether. The organic layer is separated, dried over MgSO4, concentrated in vacuo, diluted with hexane, stirred at reflux, cooled to room temperature and decanted to obtain a clear solution. The solution is concentrated in vacuo and chromatographed to give the title product.

후처리

  1. customThe organic layer is separated
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. additiondiluted with hexane
  5. temperatureat reflux
  6. temperaturecooled to room temperature
  7. customdecanted
  8. customto obtain a clear solution
  9. concentrationThe solution is concentrated in vacuo
  10. customchromatographed

출처 및 근거

ORD 기록
ord-1d804fda3f4a48829d05b874f762e3a7
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05480902

반응 노트

불러오는 중…