Sodium Hydroxide → HCID 178435087、化合物

HRID 2298690ノート

反応式

HRID 2298690 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8]([O:10]C)=[S:9])[S:5][C:6]=1[CH3:7].[OH-].[Na+]>CO.O>[Br:1][C:2]1[CH:3]=[C:4]([C:8]([OH:10])=[S:9])[S:5][C:6]=1[CH3:7]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 86583861Methyl 4-bromo-5-methylthiothiophene-2-carboxylate

生成物 1

HCID 178435087HCID 178435087、化合物収率 94.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To 1.0 g (3.7 mmol) of methyl 4-bromo-5-methylthiothiophene-2-carboxylate (as prepared in Example 241, step (a) dissolved in 25 ml of MeOH was added 450 mg of NaOH dissolved in 10 ml of H2O. The reaction was stirred for 5 hours at room temperature, and then the solvents were removed under vacuum. The residue of the reaction was extracted with ethyl acetate (2×50 mL) and 1N HCl. The organic layer was collected, dried (Na2SO4), filtered and concentrated under vacuum to yield 833 mg (89%) of 4-bromo-5-methylthiothiophene-2-carboxylic acid as a white solid.

後処理

  1. customthe solvents were removed under vacuum
  2. extractionThe residue of the reaction was extracted with ethyl acetate (2×50 mL) and 1N HCl
  3. customThe organic layer was collected
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-cfb4b2fe0a3e4295bf63c692cff55db8
出典データセット
uspto-grants-2002_12
特許番号
US06492403B1

反応ノート

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