Triethylamine → Ethyl 2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)-3-dimethylaminoacrylate

HRID 1861214

반응식

HRID 1861214 반응식
[CH3:1][N:2]([CH3:10])[CH:3]=[CH:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].C(N(CC)CC)C.[F:18][C:19]1[C:27]([CH3:28])=[C:26]([F:29])[C:25]([F:30])=[C:24]([N+:31]([O-:33])=[O:32])[C:20]=1[C:21](Cl)=[O:22]>C(OCC)(=O)C>[CH3:1][N:2]([CH3:10])[CH:3]=[C:4]([C:21](=[O:22])[C:20]1[C:24]([N+:31]([O-:33])=[O:32])=[C:25]([F:30])[C:26]([F:29])=[C:27]([CH3:28])[C:19]=1[F:18])[C:5]([O:7][CH2:8][CH3:9])=[O:6]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 121015Ethyl 3-(N,N-dimethylamino)acrylateHCID 10610913HCID 10610913, 화합물

생성물 1

HCID 72820967Ethyl 2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)-3-dimethylaminoacrylate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

반응 조건

온도
5 °C

실험 절차

1.4 g (0.01 mol) of ethyl 3-dimethylaminoacrylate, 15 ml of ethyl acetate and 1.4 ml (0.01 mol) of triethylamine were loaded and cooled to 5° C., and a liquid mixture of 3.5 g (0.011 mol) of 2,4,5-trifluoro-3-methyl-6-nitrobenzoyl chloride and 5 ml of ethyl acetate was added dropwise while the temperature was maintained at 0 to 5° C. The resulting mixture was stirred at 5° C. for 1 hour and then stirred at room temperature (25° C.) for 2 hours. The precipitated triethylamine hydrochloride was filtered off, and the filtrate was concentrated under reduced pressure to give ethyl 3-dimethylamino-2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)acrylate with a 43.6% purity as the residue.

후처리

  1. additionwas added dropwise while the temperature
  2. temperaturewas maintained at 0 to 5° C
  3. stirringstirred at room temperature (25° C.) for 2 hours
  4. filtrationThe precipitated triethylamine hydrochloride was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5be380bdb4b649f1b67b654cd9f22e37
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06531624B1

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