Potassium Hydroxide → 4,6-Diisopropoxy-2-(trifluoromethyl)-3-pyridinecarboxylic acid

HRID 1251953노트

반응식

HRID 1251953 반응식
[CH:1]([O:4][C:5]1[CH:10]=[C:9]([O:11][CH:12]([CH3:14])[CH3:13])[N:8]=[C:7]([C:15]([F:18])([F:17])[F:16])[C:6]=1[C:19]([O:21]CC)=[O:20])([CH3:3])[CH3:2].[OH-].[K+]>CO>[CH:1]([O:4][C:5]1[CH:10]=[C:9]([O:11][CH:12]([CH3:14])[CH3:13])[N:8]=[C:7]([C:15]([F:18])([F:17])[F:16])[C:6]=1[C:19]([OH:21])=[O:20])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 13726788Ethyl 4,6-diisopropoxy-2-(trifluoromethyl)-3-pyridinecarboxylate

생성물 1

HCID 137267904,6-Diisopropoxy-2-(trifluoromethyl)-3-pyridinecarboxylic acid수율 73.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 9.5 g (0.0283 mol) of product of Example 6, 10 g of KOH and 150 ml of methanol was held at reflux for 16 hours. Methanol was removed under reduced pressure. The residue was treated with 300 ml of water and extracted with ether. The aqueous layer was poured into 50 ml of concentrated HCl and extracted with ether. The ether extract was concentrated. The residue solid (7.7 g) was recrystallized from hexane-ether to give 6.4 g (73.6%) of acid product: mp 147°-150° C.

후처리

  1. temperatureat reflux for 16 hours
  2. customMethanol was removed under reduced pressure
  3. additionThe residue was treated with 300 ml of water
  4. extractionextracted with ether
  5. additionThe aqueous layer was poured into 50 ml of concentrated HCl
  6. extractionextracted with ether
  7. extractionThe ether extract
  8. concentrationwas concentrated
  9. customThe residue solid (7.7 g) was recrystallized from hexane-ether

출처 및 근거

ORD 기록
ord-c069ba56468449c6a5ac9d7b864d0933
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04741766

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