Sodium Hydroxide → 7-(2,5-Dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid

HRID 1646825

反応式

HRID 1646825 の反応式
[OH-].[Na+].[CH3:3][O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[C:7]([CH3:15])[C:6]=1[CH:16]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH2:17][CH2:18][CH2:19][CH2:20][C:21]([CH3:28])([CH3:27])[C:22]([O:24]CC)=[O:23]>C(O)C>[CH3:3][O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[C:7]([CH3:15])[C:6]=1[CH:16]([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[CH2:17][CH2:18][CH2:19][CH2:20][C:21]([CH3:28])([CH3:27])[C:22]([OH:24])=[O:23]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 19088026Ethyl 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoate

生成物 1

HCID 190880747-(2,5-Dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

3N Sodium hydroxide (9 ml) was added to a solution of 1.20 g (2.73 mmole) of ethyl 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoate in ethanol (12 ml), followed by stirring at 90° C. overnight (15 hours). After cooling by standing at room temperature, the ethanol was distilled off under reduced pressure, and the residue was made acid by adding a 10% aqueous phosphoric acid solution, followed by extraction of the product with isopropyl ether. The isopropyl ether layer was washed with aqueous sodium hydrochloride solution, dried (magnesium suflate) and evaporated to give 1.11 q (99%) of 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid. Its typical physical properties and nuclear magnetic resonance spectrum data are shown in Table 14.

後処理

  1. temperatureAfter cooling
  2. customby standing at room temperature
  3. distillationthe ethanol was distilled off under reduced pressure
  4. additionby adding a 10% aqueous phosphoric acid solution
  5. extractionfollowed by extraction of the product with isopropyl ether
  6. washThe isopropyl ether layer was washed with aqueous sodium hydrochloride solution
  7. dry with materialdried (magnesium suflate)
  8. customevaporated

出典と根拠

ORDレコード
ord-159e3818d89848a4bed8302dc9d8b313
出典データセット
uspto-grants-1993_01
特許番号
US05180742

関連ノート

読み込み中…