Sodium Hydroxide → HCID 22759245、化合物

HRID 460858ノート

反応式

HRID 460858 の反応式
[C:1]([CH:4]([CH2:16][CH2:17][CH2:18][CH:19]([OH:32])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13]CC)=[O:12])(=[O:3])[CH3:2].[OH-].[Na+]>O.CO>[C:1]([CH:4]([CH2:16][CH2:17][CH2:18][CH:19]([OH:32])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:30])([F:31])[F:29])[CH:23]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 22759220HCID 22759220、化合物

生成物 1

HCID 22759245HCID 22759245、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A solution of ethyl 8-acetyl-12-hydroxy-13-(3-trifluoromethylphenoxy)tridecanoate (17.4 g., 0.038 mole) and sodium hydroxide (4 g., 0.1 mole) in water (30 ml.) and methanol (120 ml.) is heated at 60° for 16 hours. Most of the methanol is then removed by distillation in vacuo. The residue is dissolved in 150 ml. of water and extracted with ether. The aqueous solution is acidified with concentrated hydrochloric acid. The oily product is taken up in ether and dried over sodium sulfate. Ether is evaporated in vacuo to leave the title compound as a viscous oil weighing 12.9 g. The product is purified by column chromatography on 200 g. of silica gel with 2% methanol in chloroform as eluant; pmr (CDCl3) δ 2.10 (3H, s CH3CO); 3.95 (3H, broad s CHO and CH2O); 6.75 (2H, s OH and CO2H).

後処理

  1. customMost of the methanol is then removed by distillation in vacuo
  2. dissolutionThe residue is dissolved in 150 ml
  3. extractionof water and extracted with ether
  4. dry with materialdried over sodium sulfate
  5. customEther is evaporated in vacuo

出典と根拠

ORDレコード
ord-3666abe8ade24cee92326c4a2a5b852b
出典データセット
uspto-grants-1977_12
特許番号
US04061643

反応ノート

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