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Beta-Propiolactone → HCID 20135581、化合物

HRID 579990
ノート
印刷プレビュー

反応式

HRID 579990 の反応式
[Cl:1][C:2]1[C:9]([Cl:10])=[C:8]([OH:11])[CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[C:12]1(=[O:16])[O:15][CH2:14][CH2:13]1>[OH-].[Na+].CCOCC>[Cl:10][C:9]1[C:2]([Cl:1])=[C:3]([CH:4]=[O:5])[CH:6]=[CH:7][C:8]=1[O:11][CH2:14][CH2:13][C:12]([OH:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 2365Beta-PropiolactoneHCID 5283802,3-Dichloro-4-hydroxybenzaldehyde

生成物 1

HCID 20135581HCID 20135581、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 14798Sodium Hydroxide溶媒2 回

実験手順

2,3-dichloro-4-hydroxybenzaldehyde (38.2 g., 0.2 mole) is dissolved in a 10% sodium hydroxide solution (200 ml.). The solution is heated to boiling and β-propiolactone (144 g., 2.0 moles) is added dropwise at such a rate as to keep the solution boiling. During the addition 10% sodium hydroxide solution is added in portions to maintain an alkaline mixture. Then the solution is cooled and acidified. The precipitated material is dissolved in ether and the product is extracted into a 5% sodium bicarbonate solution. Acidification of the aqueous solution precipitates 3-(2,3-dichloro-4-formylphenoxy)propionic acid, which is purified by recrystallization from ethyl acetate.

後処理

  1. additionis added dropwise at such a rate as
  2. additionis added in portions
  3. temperatureto maintain an alkaline mixture
  4. temperatureThen the solution is cooled
  5. extractionthe product is extracted into a 5% sodium bicarbonate solution
  6. customAcidification of the aqueous solution precipitates 3-(2,3-dichloro-4-formylphenoxy)propionic acid, which
  7. customis purified by recrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-34c4669876e5496c9e800ddd0ff089ff
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04751244

反応ノート

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