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Acetic Anhydride → 2-Propenoic acid, 2-(acetyloxy)-, ethyl ester

HRID 868771
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HRID 868771 반응식
[C:1]([O:6][CH2:7][CH3:8])(=[O:5])[C:2]([CH3:4])=[O:3].[C:9](OC(=O)C)(=[O:11])[CH3:10]>O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O)(=O)C>[C:9]([O:3][C:2](=[CH2:4])[C:1]([O:6][CH2:7][CH3:8])=[O:5])(=[O:11])[CH3:10]
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참가 물질

5

반응물 2

HCID 7918Acetic Anhydride2회HCID 12041Ethyl pyruvate

생성물 1

HCID 112173872-Propenoic acid, 2-(acetyloxy)-, ethyl ester수율 58.5%

시약·촉매·용매 2

HCID 521998p-Toluenesulfonic acid monohydrate촉매HCID 176Acetic Acid용매

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온도
120 °C
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실험 절차

First, to a mixture of ethyl pyruvate (315 g, 2.7 mol) and acetic anhydride (554 g, 5.4 mol), p-toluenesulfonic acid monohydrate (8 g) was added. Then, the mixture was stirred under a nitrogen gas stream at 120° C. for 24 hours to obtain a reaction solution. Next, acetic acid generated by a reaction with excess acetic anhydride under reduced pressure (40 to 50 mmHg) was removed from the reaction solution. Thereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.) to obtain ethyl α-acetoxyacrylate (250 g, yield 58%).

후처리

  1. additionwas added
  2. customto obtain a reaction solution
  3. customwas removed from the reaction solution
  4. distillationThereafter, the residue was purified by reduced pressure distillation (35 to 40 mmHg, 90 to 103° C.)

출처 및 근거

ORD 기록
ord-8145e7bb54f94012b03842a0a38f85ab
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08968975B2

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