Methyl iodide → 5-Chloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester

HRID 29384ノート

反応式

HRID 29384 の反応式
[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([OH:17])[C:9]=2[C:10]=1[CH3:11])=[O:5])[CH3:2].IC.[C:20]([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([O:17][CH3:20])[C:9]=2[C:10]=1[CH3:11])=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 687146975-Chloro-4-hydroxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester

生成物 1

HCID 687120345-Chloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester収率 94%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 5-chloro-4-hydroxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester (120 mg, 0.47 mmol) was added 0.3 mL (4.7 mmol) of iodomethane, 130 mg (2 eq) of K2CO3 and 4 mL of DMF. The mixture was stirred at room temperature overnight. The mixture was washed with brine and extracted with ethyl acetate. The combined organic solution was washed with brine and water. Removal of the solvent in vacuo gavel 19 mg (94% yield) of 5-chloro-4-methoxy-3-methyl-benzofuran-2-carboxylic acid ethyl ester as a white solid.

後処理

  1. washThe mixture was washed with brine
  2. extractionextracted with ethyl acetate
  3. washThe combined organic solution was washed with brine and water

出典と根拠

ORDレコード
ord-ca8c8c18006a4cc6a15b6364c4e26db5
出典データセット
uspto-grants-2008_09
特許番号
US07420001B2

反応ノート

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