Sodium Hydroxide → Oxindanac

HRID 1438925ノート

反応式

HRID 1438925 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 crystallized 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 crystallized from ethanol-petroleum ether

出典と根拠

ORDレコード
ord-7b2cf0fbcf974122a0e62eeb598eda15
出典データセット
uspto-grants-1977_11
特許番号
US04057573

反応ノート

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