Ethyl Acrylate → HCID 68706213、化合物

HRID 2069312ノート

反応式

HRID 2069312 の反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)=[N:6][CH:7]=1.P.[CH2:16]([O:18][C:19](=[O:22])[CH:20]=[CH2:21])[CH3:17]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(N(CC)CC)C>[CH2:16]([O:18][C:19](=[O:22])[CH:20]=[CH:21][C:2]1[CH:7]=[N:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1)[CH3:17]

参加物

6

反応物 3

HCID 8821Ethyl AcrylateHCID 24404PhosphineHCID 221807795-Bromo-2-(4-fluorophenyl)pyridine

生成物 1

HCID 68706213HCID 68706213、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
90 °C

実験手順

9.30 g (36.9 mmol) of 5-bromo-2-(4-fluoro-phenyl)-pyridine were mixed with 100 ml of triethylamine, 2.06 g (9.2 mmol) of palladium acetate, 2.80 g (9.2 mmol) of tri)ortho-tolyl)phosphine and 6.47 g (64.6 mmol) of acrylic acid ethyl ester and heated to 90° C. for 2 h. The reaction mixture was evaporated, taken up in water and extracted with ethyl acetate. The combined organic phases were dried and evaporated, and the residue was subjected to column chromatography (silica gel, n-heptane/ethyl acetate 3:1). Yield: 7.7 g.

後処理

  1. customThe reaction mixture was evaporated
  2. extractionextracted with ethyl acetate
  3. customThe combined organic phases were dried
  4. customevaporated

出典と根拠

ORDレコード
ord-d159d3ba97454be6a663c475ee9ec488
出典データセット
uspto-grants-2012_10
特許番号
US08299102B2

反応ノート

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