Sodium Hydroxide → Oxindanac

HRID 1680264ノート

反応式

HRID 1680264 の反応式
C[O:2][C:3]([CH:5]1[C:13]2[C:8](=[CH:9][C:10]([C:15](=[O:22])[C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[C:11]([OH:14])[CH:12]=2)[CH2:7][CH2:6]1)=[O:4].[OH-].[Na+]>CO>[C:15]([C:10]1[CH:9]=[C:8]2[C:13](=[CH:12][C:11]=1[OH:14])[CH:5]([C:3]([OH:4])=[O:2])[CH2:6][CH2:7]2)(=[O:22])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 54109752HCID 54109752、化合物

生成物 1

HCID 68879Oxindanac

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 8.2 g of 5-benzoyl-6-hydroxy-indane-1-carboxylic acid methyl ester in 150 ml of methanol is mixed with 20 ml of 2 N sodium hydroxide solution and the mixture is boiled for 3 hours under reflux. It is then evaporated to dryness in vacuo and the evaporation residue is partitioned between 100 ml of 2 N hydrochloric acid and 3 times 100 ml of methylene chloride. The organic phases are washed until neutral, dried over sodium sulphate, treated with active charcoal and evaporated in vacuo. The evaporation residue, when crystallised from ethanol-petroleum ether, gives 5-benzoyl-6-hydroxy-indane-1-carboxylic acid in the form of yellow platelets of melting point 185°-7° C.

後処理

  1. temperatureunder reflux
  2. customIt is then evaporated to dryness in vacuo
  3. customthe evaporation residue is partitioned between 100 ml of 2 N hydrochloric acid and 3 times 100 ml of methylene chloride
  4. washThe organic phases are washed until neutral,
  5. dry with materialdried over sodium sulphate
  6. additiontreated with active charcoal
  7. customevaporated in vacuo
  8. customThe evaporation residue, when crystallised from ethanol-petroleum ether

出典と根拠

ORDレコード
ord-f72d2054917240deab89c4635db292f1
出典データセット
uspto-grants-1981_06
特許番号
US04272547

反応ノート

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