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Beta-Propiolactone → HCID 20135581, 화합물

HRID 579990
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HRID 579990 반응식
[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]
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참가 물질

5

반응물 2

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

생성물 1

HCID 20135581HCID 20135581, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 14798Sodium Hydroxide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-34c4669876e5496c9e800ddd0ff089ff
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04751244

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