Water → 4-methylbenzoic acid [(R)-2-methylheptyl]ester

HRID 1033130

反応式

HRID 1033130 の反応式
C[C@@H:2](O)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH3:10][C:11]1[CH:19]=[CH:18][C:14]([C:15](Cl)=[O:16])=[CH:13][CH:12]=1.[OH2:20].[C:21]1(C)C=CC=CC=1>N1C=CC=CC=1>[CH3:21][C@H:7]([CH2:6][CH2:5][CH2:4][CH2:3][CH3:2])[CH2:8][O:20][C:15](=[O:16])[C:14]1[CH:18]=[CH:19][C:11]([CH3:10])=[CH:12][CH:13]=1

参加物

6

反応物 4

HCID 962WaterHCID 1140TolueneHCID 134054-Methylbenzoyl ChlorideHCID 80080(R)-2-Octanol

生成物 1

HCID 540413924-methylbenzoic acid [(R)-2-methylheptyl]ester

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

40 g (0.31 moles) of a commercially available (R)-2-octanol was dissolved in 100 ml of pyridine. The mixture was cooled and 47.93 g (0.31 moles) of a commercially available 4-methylbenzoic chloride was added thereto while cooling. The mixture was then allowed to react with stirring at 50° to 60° C. for 2 hours. On completion of the reaction, 300 ml of water and 300 ml of toluene were added, and after vigorous stirring, the toluene layer was separated out and washed with 6N HCl. Washing was continued until this layer was neutral. This toluene layer was dried with anhydrous magnesium sulfate, after which the toluene was distilled away. The residue was further subjected to evaporation under reduced pressure at 144° to 146° C. (2 mm Hg) and the distillate recovered, whereby 70.37 g of the objective 4-methylbenzoic acid [(R)-2-methylheptyl] ester was obtained.

後処理

  1. temperatureThe mixture was cooled
  2. temperaturewhile cooling
  3. customto react
  4. additionwere added
  5. customafter vigorous stirring, the toluene layer was separated out and
  6. washwashed with 6N HCl
  7. washWashing
  8. dry with materialThis toluene layer was dried with anhydrous magnesium sulfate
  9. distillationafter which the toluene was distilled away
  10. customThe residue was further subjected to evaporation under reduced pressure at 144° to 146° C. (2 mm Hg)
  11. distillationthe distillate recovered

出典と根拠

ORDレコード
ord-04101fa9b45d48948f0742a43419a780
出典データセット
uspto-grants-1994_05
特許番号
US05310503

関連ノート

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