Methyl 3-iodobenzoate → Methyl 3-ethylbenzoate

HRID 4974

反応式

HRID 4974 の反応式
I[C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].[CH:12]([Sn](CCCC)(CCCC)CCCC)=[CH2:13].[F-].[K+]>C1(C)C=CC=CC=1.O.C(OCC)(=O)C.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>[CH2:12]([C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6])[CH3:13]

参加物

8

反応物 3

HCID 69258Methyl 3-iodobenzoateHCID 81998TributylvinyltinHCID 522689Potassium Fluoride

生成物 1

HCID 12430992Methyl 3-ethylbenzoate

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Methyl 3-iodobenzoate (13 g) and vinyl tributyltin (20 g) were dissolved in toluene (100 ml) and tetrakis(triphenylphosphine)palladium (0) (500 mg) added. The solution was heated at reflux with stirring under N2 for 1 day. Potassium fluoride (3 g) in water (50 ml) was added and the reaction mixture was allowed to stir under N2 for 15 minutes. The product was taken up in ethyl acetate and washed with water and then brine (×2). The organic extract was dried (MgSO4) and evaporated in vacuo.

後処理

  1. temperatureThe solution was heated
  2. temperatureat reflux
  3. stirringto stir under N2 for 15 minutes
  4. washwashed with water
  5. extractionThe organic extract
  6. dry with materialwas dried (MgSO4)
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-2bbab0f4ae63457f992a8d6c141b0c62
出典データセット
uspto-grants-1993_09
特許番号
US05242930

関連ノート

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