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Potassium Hydroxide → 2,5-Bis-(6-hydroxyhexoxy)terephthalic acid

HRID 378497
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HRID 378497 반응식
[OH-].[K+].C([O:5][C:6](=[O:40])[C:7]1[CH:17]=[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][O:25]C(=O)C)[C:10]([C:11]([O:13]CC)=[O:12])=[CH:9][C:8]=1[O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][O:36]C(=O)C)C>O.C(O)C>[OH:36][CH2:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][O:29][C:8]1[CH:9]=[C:10]([C:11]([OH:13])=[O:12])[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][OH:25])=[CH:17][C:7]=1[C:6]([OH:40])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 19354093Diethyl-2,5-bis-(6-acetoxyhexoxy)terephthalate

생성물 1

HCID 193540872,5-Bis-(6-hydroxyhexoxy)terephthalic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 25.0 g (379 mmol) 85% KOH in 300 ml water is added to 40.0 g (74.3 mmol) diethyl-2,5-bis-(6-acetoxyhexoxy)terephthalate in 250 ml ethanol and the whole is heated under reflux for 1.5 hours. After distilling off approx. 150 ml ethanol, the reaction mixture is acidified by adding 40.0 g conc. HCl and stored at 2° C. for 20 hours for complete crystallization of the crude product. The colourless crude product is then filtered off, washed neutral with water and recrystallized from ethanol.

후처리

  1. temperaturethe whole is heated
  2. temperatureunder reflux for 1.5 hours
  3. distillationAfter distilling off approx. 150 ml ethanol
  4. additionby adding 40.0 g conc. HCl
  5. customstored at 2° C. for 20 hours for complete crystallization of the crude product
  6. filtrationThe colourless crude product is then filtered off
  7. washwashed neutral with water
  8. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-e6d408f1996043e69a3e2d15a8818465
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06031015

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