Ethyl Acrylate → HCID 86649425, 화합물

HRID 1519894노트

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HRID 1519894 반응식
Br[C:2]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[C:6]([F:13])=[CH:5][C:3]=1[NH2:4].CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.[C:36]([O:40][CH2:41][CH3:42])(=[O:39])[CH:37]=[CH2:38]>C(N(CC)CC)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[NH2:4][C:3]1[CH:5]=[C:6]([F:13])[C:7]([C:9]([F:12])([F:11])[F:10])=[CH:8][C:2]=1/[CH:38]=[CH:37]/[C:36]([O:40][CH2:41][CH3:42])=[O:39]

참가 물질

6

반응물 3

HCID 8821Ethyl AcrylateHCID 80271Tri-o-tolylphosphineHCID 687591875-Fluoro-2-iodo-4-trifluoromethyl-phenylamine

생성물 1

HCID 86649425HCID 86649425, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 8471Triethylamine용매

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온도
85 °C

실험 절차

2-Bromo-5-fluoro-4-(trifluoromethyl)aniline (0.97 mmol) and P(o-tol)3 (0.40 mmol) were dissolved in triethylamine (2.0 mL) in a glass pressure tube and nitrogen gas was bubbled through the solution via a gas dispersion tube for 10 minutes. Ethyl acrylate (1.0 mmol) and palladium acetate (0.20 mmol) were added to the reaction mixture and the tube was sealed and placed into an oil bath pre-heated to 85° C. for 18 h. The resulting solution was concentrated under vacuum and purified via an isco column. Retention time (min)=2.504, method [1], MS(ESI) 278.0 (M+H).

후처리

  1. customnitrogen gas was bubbled through the solution via a gas dispersion tube for 10 minutes
  2. customthe tube was sealed
  3. customplaced into an oil bath
  4. concentrationThe resulting solution was concentrated under vacuum
  5. custompurified via an isco column

출처 및 근거

ORD 기록
ord-9e424970fb774eff9c9f4cc71a0dc223
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073891B2

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