Acetic Anhydride → HCID 14984434、化合物

HRID 868773

反応式

HRID 868773 の反応式
[C:1]([O:6][CH2:7][CH2:8][CH2:9][CH3:10])(=[O:5])[C:2]([CH3:4])=[O:3].[C:11](OC(=O)C)(=[O:13])[CH3:12]>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)(=O)C>[C:11]([O:3][C:2](=[CH2:4])[C:1]([O:6][CH2:7][CH2:8][CH2:9][CH3:10])=[O:5])(=[O:13])[CH3:12]

参加物

5

反応物 2

HCID 7918Acetic Anhydride2 回HCID 523883Butyl pyruvate

生成物 1

HCID 14984434HCID 14984434、化合物収率 67.1%

試薬・触媒・溶媒 2

HCID 521998p-Toluenesulfonic acid monohydrate触媒HCID 176Acetic Acid溶媒

反応条件

温度
120 °C

実験手順

Next, in a mixture of the obtained butyl pyruvate (235 g, 1.6 mol) and acetic anhydride (333 g, 3.3 mol), p-toluenesulfonic acid monohydrate (5 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 25 hours to obtain a second reaction solution. Next, acetic acid generated by a reaction with excess acetic anhydride under reduced pressure (5 mmHg) was removed from the second reaction solution. Thereafter, the residue was purified by reduced pressure distillation (2 mmHg, 56 to 63° C.) to obtain butyl α-acetoxyacrylate (200 g, yield 67%).

後処理

  1. additionwas added
  2. customto obtain a second reaction solution
  3. customwas removed from the second reaction solution
  4. distillationThereafter, the residue was purified by reduced pressure distillation (2 mmHg, 56 to 63° C.)

出典と根拠

ORDレコード
ord-c044d2a1fa244dfd88caa39a2fce939c
出典データセット
uspto-grants-2015_03
特許番号
US08968975B2

関連ノート

読み込み中…