Potassium Carbonate → 4-Iodo-3-(2-m-tolyl-ethoxy)-benzoic Acid Methyl Ester

HRID 1918330ノート

反応式

HRID 1918330 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([I:10])=[C:6]([OH:11])[CH:5]=1.Br[CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([I:10])=[C:6]([O:11][CH2:14][CH2:15][C:16]2[CH:17]=[C:18]([CH3:22])[CH:19]=[CH:20][CH:21]=2)[CH:5]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 5706841-(2-Bromoethyl)-3-methylbenzeneHCID 10378812Methyl 3-hydroxy-4-iodobenzoate

生成物 1

HCID 671709004-Iodo-3-(2-m-tolyl-ethoxy)-benzoic Acid Methyl Ester収率 32.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

10.0 g of 3-hydroxy-4-iodo-benzoic acid methyl ester, 7.2 g of 1-(2-bromo-ethyl)-3-methyl-benzene and 10.0 g of potassium carbonate were stirred in 100 ml of anhydrous DMF for 28 h at 80° C. The solvent was evaporated and the residue dissolved in 200 ml of water and 400 ml of EA. The organic layer was separated, washed with 200 ml of water, dried with magnesium sulfate and evaporated. Silica gel chromatography (EA/HEP gradient) of the residue yielded 4.66 g of the title compound.

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in 200 ml of water
  3. customThe organic layer was separated
  4. washwashed with 200 ml of water
  5. dry with materialdried with magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-7677469dbede4e259c64bcf03db28a03
出典データセット
uspto-grants-2013_12
特許番号
US08618304B2

反応ノート

読み込み中…