Hydrochloric Acid → 2,5-Bis-(10-hydroxydecoxy)terephthalic acid

HRID 378500노트

반응식

HRID 378500 반응식
[OH-].[K+].C([O:5][C:6](=[O:48])[C:7]1[CH:17]=[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][O:29]C(=O)C)[C:10]([C:11]([O:13]CC)=[O:12])=[CH:9][C:8]=1[O:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][O:44]C(=O)C)C.Cl>O.C(O)C>[OH:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39][CH2:38][CH2:37][CH2:36][CH2:35][CH2:34][O:33][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][CH2:25][CH2:26][CH2:27][CH2:28][OH:29])=[CH:17][C:7]=1[C:6]([OH:48])=[O:5]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 19354086Diethyl-2,5-bis-(10-acetoxydecoxy)terephthalate

생성물 1

HCID 193540842,5-Bis-(10-hydroxydecoxy)terephthalic acid

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 20.0 g (303 mmol) 85% aqueous KOH in 200 ml water is added to 38.0 g (58.4 mmol) diethyl-2,5-bis-(10-acetoxydecoxy)terephthalate in 200 ml ethanol and the whole is heated under reflux for 1.5 hours. 28.0 ml conc. HCl are then added dropwise with ice-cooling and stirring until the solution shows an acidic pH. The precipitated, colourless crude product is filtered off, washed neutral and recrystallized from ethanol and methanol/acetone.

후처리

  1. temperaturethe whole is heated
  2. temperatureunder reflux for 1.5 hours
  3. temperaturecooling
  4. filtrationThe precipitated, colourless crude product is filtered off
  5. washwashed neutral
  6. customrecrystallized from ethanol and methanol/acetone

출처 및 근거

ORD 기록
ord-0261dc4412834aa6b2f1b69ea546e9a6
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06031015

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