Sodium Hydroxide → 2-(Carboxymethyl)thiophene-3-carboxylic acid

HRID 270643

反応式

HRID 270643 の反応式
C[O:2][C:3]([CH2:5][C:6]1[S:7][CH:8]=[CH:9][C:10]=1[C:11]([O:13]C)=[O:12])=[O:4].[OH-].[Na+]>CO.O>[C:3]([CH2:5][C:6]1[S:7][CH:8]=[CH:9][C:10]=1[C:11]([OH:13])=[O:12])([OH:4])=[O:2]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 58952963Methyl 2-(2-methoxy-2-oxoethyl)thiophene-3-carboxylate

生成物 1

HCID 206212852-(Carboxymethyl)thiophene-3-carboxylic acid収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

13.0 g of the compound obtained in Example 1 was dissolved in 260 mL of methanol, and a solution obtained by dissolving 4.84 g of sodium hydroxide in 26 mL of water was added thereto. The resulting solution was refluxed for 4 hours, cooled to room temperature, concentrated under reduced pressure to remove methanol. The resulting aqueous solution was washed with 10 ml of diethyl ether and acidified to pH 2 to 3 using concentrated HCl. The solids thus solidified were filtered, washed with a small amount of cold water and dried at 40° C. to obtain 9.60 g (yield of 85%) of the title compound as a brown solid.

後処理

  1. customa solution obtained
  2. additionwas added
  3. temperatureThe resulting solution was refluxed for 4 hours
  4. concentrationconcentrated under reduced pressure
  5. customto remove methanol
  6. washThe resulting aqueous solution was washed with 10 ml of diethyl ether
  7. filtrationThe solids thus solidified were filtered
  8. washwashed with a small amount of cold water
  9. customdried at 40° C.

出典と根拠

ORDレコード
ord-0f920847adf342cfad86735dfee72b9c
出典データセット
uspto-grants-2008_11
特許番号
US07449580B2

関連ノート

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