Hydrochloric Acid → 2-{5-[(2,4-Diisobutoxyphenyl)(hydroxy)methyl]-2-isobutoxyphenyl}-acetic acid

HRID 2249616ノート

反応式

HRID 2249616 の反応式
[CH2:1]([O:5][C:6]1[CH:28]=[C:27]([O:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH:26]=[CH:25][C:7]=1[C:8]([C:10]1[CH:11]=[CH:12][C:13]([O:20][CH2:21][CH:22]([CH3:24])[CH3:23])=[C:14]([CH2:16][C:17]([OH:19])=[O:18])[CH:15]=1)=[O:9])[CH:2]([CH3:4])[CH3:3].[BH4-].[Na+].[Cl-].[Li+].Cl>CO.O.C(Cl)(Cl)Cl>[CH2:1]([O:5][C:6]1[CH:28]=[C:27]([O:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH:26]=[CH:25][C:7]=1[CH:8]([OH:9])[C:10]1[CH:11]=[CH:12][C:13]([O:20][CH2:21][CH:22]([CH3:24])[CH3:23])=[C:14]([CH2:16][C:17]([OH:19])=[O:18])[CH:15]=1)[CH:2]([CH3:4])[CH3:3]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 433294Lithium ChlorideHCID 4311764Sodium borohydride2 回HCID 178165642-[5-(2,4-Diisobutoxybenzoyl)-2-isobutoxyphenyl]acetic acid

生成物 1

HCID 576843802-{5-[(2,4-Diisobutoxyphenyl)(hydroxy)methyl]-2-isobutoxyphenyl}-acetic acid収率 49.8%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6212Chloroform溶媒

反応条件

温度
55 °C

実験手順

In 2 ml of methanol is dissolved 100 mg of 2-[5-(2,4-diisobutoxybenzoyl)-2-isobutoxyphenyl]acetic acid. After adding 18 mg of sodium borohydride at 5-10° C., the mixture thus obtained is stirred at 50-60° C. for one hour. Then, 40 mg of sodium borohydride and 40 mg of lithium chloride are further added at ambient temperature, and the mixture thus obtained is stirred at 50-60° C. for two hours. Chloroform and water are added to the reaction mixture, pH is adjusted to 2.0 with 2 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is successively washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. Thus, 50 mg of 2-{5-[(2,4-diisobutoxyphenyl)(hydroxy)methyl]-2-isobutoxyphenyl}-acetic acid is obtained as a colorless oily product.

後処理

  1. customthe mixture thus obtained
  2. customthe mixture thus obtained
  3. stirringis stirred at 50-60° C. for two hours
  4. customthe organic layer is separated
  5. washThe organic layer is successively washed with water and saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4925ea3363ae4cd391512edc94ca8433
出典データセット
uspto-grants-2008_01
特許番号
US07314888B1

反応ノート

読み込み中…