Acetic Anhydride → 3-Methyl-2-nonen-1-YL acetate

HRID 1863148

反応式

HRID 1863148 の反応式
[CH3:1][C:2]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])=[CH:3][CH2:4][OH:5].[C:12](OC(=O)C)(=[O:14])[CH3:13].C(O)(=O)C.C1(C)C=CC=CC=1>C1(C)C=CC=CC=1.C(O)(=O)C>[C:12]([O:5][CH2:4][CH:3]=[C:2]([CH3:1])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])(=[O:14])[CH3:13]

参加物

6

反応物 3

HCID 7918Acetic AnhydrideHCID 2309923-Methyl-2-nonen-1-olHCID 18331056Acetic acid toluene

生成物 1

HCID 736775943-Methyl-2-nonen-1-YL acetate

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 1140Toluene溶媒2 回

実験手順

156 G. (1 mole) of 3-methyl-2-nonen-1-ol, 122 g. (1.2 moles) of acetic anhydride and 264 ml. of toluene were combined in a reaction flask and heated. The formed acetic acid-toluene azeotropic mixture consisting of 34 parts of acetic acid and 66 parts of toluene and boiling at 105° C. was removed by distillation through a 11/2 ft. Vigreux column. After termination of the reaction, the reaction mass was washed with 100 ml. of aqueous sodium carbonate solution, 100 ml. of aqueous sodium bicarbonate solution, and finally twice with 100 ml. of water. The desired ester, 3-methyl-2-nonen-1-yl-acetate, having a b.p. of 119°-121° C. at 10 mm. and an R.I. at 20°:1.445, was recovered by fractional distillation.

後処理

  1. temperatureheated
  2. customwas removed by distillation through a 11/2 ft
  3. customAfter termination of the reaction
  4. washthe reaction mass was washed with 100 ml
  5. distillationat 20°:1.445, was recovered by fractional distillation

出典と根拠

ORDレコード
ord-da442f35ed4c43b0b262f172a07f7e47
出典データセット
uspto-grants-1979_09
特許番号
US04168248

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