Sodium Hydroxide → 5-Bromo-6-methoxybenzo[b]thiophene-3-carboxylic acid

HRID 581982ノート

反応式

HRID 581982 の反応式
[Br:1][C:2]1[C:15]([O:16][CH3:17])=[CH:14][C:5]2[S:6][CH:7]=[C:8]([C:9]([O:11]CC)=[O:10])[C:4]=2[CH:3]=1.[OH-].[Na+]>C(O)C.O>[Br:1][C:2]1[C:15]([O:16][CH3:17])=[CH:14][C:5]2[S:6][CH:7]=[C:8]([C:9]([OH:11])=[O:10])[C:4]=2[CH:3]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 53817228Ethyl 5-bromo-6-methoxybenzo[b]thiophene-3-carboxylate

生成物 1

HCID 537810295-Bromo-6-methoxybenzo[b]thiophene-3-carboxylic acid収率 96.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Ethyl 5-bromo-6-methoxybenzo[b]thiophene-3-carboxylate (D4) (0.42 g, 0.0013 mole) in ethanol (20 ml) and water (5 ml) was treated with sodium hydroxide powder (0.14 g, 0.0035 mole). The reaction mixture was heated under reflux for 2 hours and stirred at ambient temperature for 16 hours. The solvent was removed in vacuo and the residue diluted with water (25 ml), acidified with 5N hydrochloric acid, extracted into ethyl acetate, dried (Na2SO4) and evaporated in vacuo to afford the title compound (0.36 g, 93%) as a beige solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 2 hours
  3. customThe solvent was removed in vacuo
  4. additionthe residue diluted with water (25 ml)
  5. extractionextracted into ethyl acetate
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-212c164fe6a64f7fbed576362b4b2f64
出典データセット
uspto-grants-1999_07
特許番号
US05922733

反応ノート

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