Ethyl Acrylate → HCID 86649425、化合物

HRID 2098107ノート

反応式

HRID 2098107 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 86649425HCID 86649425、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 8471Triethylamine溶媒

反応条件

温度
85 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a308a17fabc04b1f90663cbd83492762
出典データセット
uspto-grants-2013_05
特許番号
US08450363B2

反応ノート

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