Allyltributylstannane → HCID 59633949、化合物

HRID 1615077ノート

反応式

HRID 1615077 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:3]=1.[CH2:13]([Sn](CCCC)(CCCC)CCCC)[CH:14]=[CH2:15]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:15]([C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:3]=1)[CH:14]=[CH2:13]

参加物

5

反応物 2

HCID 90628AllyltributylstannaneHCID 130153594-Chloropyridine-2-carboxylic acid ethyl ester

生成物 1

HCID 59633949HCID 59633949、化合物収率 73%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

To a solution of ethyl 4-chloropyridin-2-carboxylate (0.37 g) and allyltributyltin (IV) (0.86 mL) in toluene (5.0 mL) was added tetrakis(triphenylphosphine)palladium (0) (0.12 g). The reaction mixture was stirred under nitrogen atmosphere at 120° C. for 12 hr. The solvent of the reaction mixture was removed under reduced pressure. The residue was purified by silica gel chromatography (Developing solvent: hexane/ethyl acetate=3/2) to give the title compound (0.28 g, 73%).

後処理

  1. customThe solvent of the reaction mixture was removed under reduced pressure
  2. customThe residue was purified by silica gel chromatography (Developing solvent: hexane/ethyl acetate=3/2)

出典と根拠

ORDレコード
ord-9aeda1891f754190a23b6ed7b3aba932
出典データセット
uspto-grants-2014_07
特許番号
US08765739B2

反応ノート

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