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Sulfuric Acid → 1-Methylethyl (2E)-2-butenoate

HRID 881776
ノート
印刷プレビュー

反応式

HRID 881776 の反応式
[C:1]([OH:6])(=[O:5])/[CH:2]=[CH:3]/[CH3:4].[CH3:7][CH:8](O)[CH3:9].S(=O)(=O)(O)O>>[CH:8]([O:5][C:1](=[O:6])/[CH:2]=[CH:3]/[CH3:4])([CH3:9])[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 3776IsopropanolHCID 637090Crotonic Acid

生成物 1

HCID 53543591-Methylethyl (2E)-2-butenoate収率 76.3%

実験手順

Crotonic acid (193.7 g, 2.25 mol) was dissolved in 2-propanol (860 mL, 11.25 mol) in a 2 L flask and then well stirred, after which sulfuric acid (24 mL, 0.45 mol) was slowly added in droplets to the mixture and refluxed and stirred for 48 hours or longer. The stirred mixture was cooled to room temperature, after which the obtained mixture was washed with distilled water (1000 mL), and the organic layer was separated, neutralized and subjected to atmospheric distillation (80° C.), thus obtaining 220 g (1.71 mol, yield 76.3%) of crotonic acid isopropyl ester.

後処理

  1. temperaturerefluxed
  2. stirringstirred for 48 hours or longer
  3. washafter which the obtained mixture was washed with distilled water (1000 mL)
  4. customthe organic layer was separated
  5. distillationsubjected to atmospheric distillation (80° C.)

出典と根拠

ORDレコード
ord-0db0de5db94641a48e202ca03664dc84
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993694B2

反応ノート

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