Hydrochloric Acid → 3,4-Bis(heptyloxy)benzoic acid

HRID 248013ノート

反応式

HRID 248013 の反応式
C[O:2][C:3](=[O:26])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])=[C:6]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH:5]=1.[OH-].[K+].O.Cl>C(O)C>[CH2:19]([O:18][C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[C:3]([OH:26])=[O:2])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14797Potassium HydroxideHCID 540951973,4-Bis(heptyloxy)benzoic acid methyl ester

生成物 1

HCID 190152233,4-Bis(heptyloxy)benzoic acid収率 93.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 25 g of product from Example 109, 11.54 g of potassium hydroxide, 30 ml of water and 500 ml ethyl alcohol is heated at reflux temperature for 24 hours. The reaction mixture is cooled and maintained at room temperature for 48 hours. The mixture is acidified to pH 2 with concentrated hydrochloric acid, concentrated in vacuo, diluted with water and extracted with chloroform. The combined chloroform extracts are washed with saturated sodium chloride, dried and concentrated in vacuo to give 22.58 g of the desired product as colorless crystals.

後処理

  1. temperatureis heated
  2. temperatureat reflux temperature for 24 hours
  3. temperatureThe reaction mixture is cooled
  4. concentrationconcentrated in vacuo
  5. additiondiluted with water
  6. extractionextracted with chloroform
  7. washThe combined chloroform extracts are washed with saturated sodium chloride
  8. customdried
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7d4d19d8acd544a18e237dcf5b24b335
出典データセット
uspto-grants-1993_05
特許番号
US05208247

反応ノート

読み込み中…