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Dimethylformamide → Methyl 2-ethoxy-4-iodobenzoate

HRID 531038
ノート
印刷プレビュー

反応式

HRID 531038 の反応式
I[CH2:2][CH3:3].[OH:4][C:5]1[CH:14]=[C:13]([I:15])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8].C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>O>[CH2:2]([O:4][C:5]1[CH:14]=[C:13]([I:15])[CH:12]=[CH:11][C:6]=1[C:7]([O:9][CH3:10])=[O:8])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 11380407Methyl 4-iodosalicylate

生成物 1

HCID 66635397Methyl 2-ethoxy-4-iodobenzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Iodoethane (6.47 mL) was added to a mixture of methyl 2-hydroxy-4-iodobenzoate (15 g), potassium carbonate (14.9 g), and DMF (100 mL), and the resultant mixture was stirred at 70° C. for 1 hour in a nitrogen atmosphere. Water was added to the reaction mixture at room temperature, followed by extraction with ethyl acetate. The obtained organic layer was washed with saturated saline and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (16.5 g).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe obtained organic layer was washed with saturated saline
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-db17a1da3744405ca66873a9eee24286
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353108B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート