Sodium Hydroxide → 2-Thioanisylterepthalic acid

HRID 1493853

反応式

HRID 1493853 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:19]=[C:18]([C:20]([O:22]C)=[O:21])[CH:17]=[CH:16][C:11]=1[C:12]([O:14]C)=[O:13].[OH-].[Na+]>CO>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH3:9])=[CH:4][C:3]=1[C:10]1[CH:19]=[C:18]([C:20]([OH:22])=[O:21])[CH:17]=[CH:16][C:11]=1[C:12]([OH:14])=[O:13]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 86744855Dimethyl 2-thioanisylterepthalate

生成物 1

HCID 867448562-Thioanisylterepthalic acid収率 76.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Dimethyl 2-thioanisylterepthalate (3.92 g) was suspended in methanol (45.9 ml), 5M NaOH (13.5 ml) was added. The reaction mixture was heated at reflux for 1.5 hours. The methanol was removed under reduced pressure. The residues was treated with ethyl acetate and water and the layers separated. The aqueous layer was washed once with ethyl acetate. The aqueous layer was then acidified with 2N HCl and extracted three times with ethyl acetate. These combined organic extracts were then dried over MgSO4, filtered and evaporated under reduced pressure gave the product (2.75 g).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. customThe methanol was removed under reduced pressure
  4. additionThe residues was treated with ethyl acetate and water
  5. customthe layers separated
  6. washThe aqueous layer was washed once with ethyl acetate
  7. extractionextracted three times with ethyl acetate
  8. dry with materialThese combined organic extracts were then dried over MgSO4
  9. filtrationfiltered
  10. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-33a65fa02cbb4174b5332c5dfe3cf5fe
出典データセット
uspto-grants-1991_06
特許番号
US05025007

関連ノート

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