2-Chloro-N,N-dimethylethylamine → 2-(p-Isobutylphenyl)propionic acid dimethylaminoethyl ester

HRID 26447

反応式

HRID 26447 の反応式
[Na+].[CH2:2]([C:6]1[CH:11]=[CH:10][C:9]([CH:12]([CH3:16])[C:13]([O-:15])=[O:14])=[CH:8][CH:7]=1)[CH:3]([CH3:5])[CH3:4].[CH3:17][N:18]([CH2:20][CH2:21]Cl)[CH3:19]>C1C=CC=CC=1>[CH3:17][N:18]([CH2:20][CH2:21][O:14][C:13](=[O:15])[CH:12]([C:9]1[CH:8]=[CH:7][C:6]([CH2:2][CH:3]([CH3:5])[CH3:4])=[CH:11][CH:10]=1)[CH3:16])[CH3:19]

参加物

4

反応物 2

HCID 79012-Chloro-N,N-dimethylethylamineHCID 5338317Ibuprofen, Sodium Salt

生成物 1

HCID 136019482-(p-Isobutylphenyl)propionic acid dimethylaminoethyl ester収率 87.3%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 3.3 g of 2-(p-isobutylphenyl)propionic acid sodium salt, 2.3 g of dimethylaminoethyl chloride and 30 ml of benzene was refluxed for 12 hours. A solid mass produced was filtered off, and the benzene was distilled away from the filtrate under reduced pressure to leave an oily residue. This redidue was distilled under reduced pressure to give 3.5 g of 2-(p-isobutylphenyl)propionic acid dimethylaminoethyl ester as a colorless oil, boiling at 133°-136° C./1 mmHg. Analysis-Calculated for C17H27NO2 : C, 73.61; H, 9.81; N, 5.05. Found: C, 73.50; H, 9.72; N, 5.02. The infrared spectrum showed strong C=O absorption at 1730 cm-1 characteristic for ester. Mass spectrum: parent ion 277 m/e.

後処理

  1. temperaturewas refluxed for 12 hours
  2. customA solid mass produced
  3. filtrationwas filtered off
  4. distillationthe benzene was distilled away from the filtrate under reduced pressure
  5. customto leave an oily residue
  6. distillationThis redidue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-ef2503e9a937472aafda45fcee7cd763
出典データセット
uspto-grants-1979_04
特許番号
US04150137

関連ノート

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