Sodium Hydroxide → 2-(9H-fluoren-9-yloxy)acetic acid

HRID 1729246ノート

反応式

HRID 1729246 の反応式
[OH-].[Na+].[CH:3]1[C:15]2[CH:14]([O:16][CH2:17][C:18]([O:20]CC)=[O:19])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7]=2[CH:6]=[CH:5][CH:4]=1>C(O)C>[CH:12]1[C:13]2[CH:14]([O:16][CH2:17][C:18]([OH:20])=[O:19])[C:15]3[C:7](=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:8]=2[CH:9]=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 19011665Ethyl 9-fluorenyloxyacetate

生成物 1

HCID 190116622-(9H-fluoren-9-yloxy)acetic acid収率 86.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

10 ml of 1N sodium hydroxide was added dropwise to a solution of 2.28 g of ethyl 9-fluorenyloxyacetate in 40 ml of ethanol, and the mixture was stirred at room temperature for 4 hours. The reaction mixture was concentrated and water was added. After washing with ether, the pH value of the aqueous layer was adjusted with 18% hydrochloric acid to 3 to 4 under ice-cooling, followed by extraction with ether. The organic layer was dried over anhydrous magnesium sulfate, and concentrated to give 1.77 g of 9-fluorenyloxyacetic acid.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionwater was added
  3. washAfter washing with ether
  4. temperaturecooling
  5. extractionfollowed by extraction with ether
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-d314def3ad9140b6b83d53df58b3dd8a
出典データセット
uspto-grants-1994_07
特許番号
US05332734

反応ノート

読み込み中…