Hydrochloric Acid → DH 990

HRID 596988

반응식

HRID 596988 반응식
[C:1]([C:5]1[CH:6]=[C:7]([S:16][CH:17]([CH2:23][CH2:24][CH2:25][CH3:26])[C:18]([O:20]CC)=[O:19])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[OH-].[K+].Cl>C(O)C>[C:12]([C:9]1[CH:8]=[C:7]([S:16][CH:17]([CH2:23][CH2:24][CH2:25][CH3:26])[C:18]([OH:20])=[O:19])[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[C:10]=1[OH:11])([CH3:13])([CH3:14])[CH3:15]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 21449469Ethyl 2-((3,5-di-tert-butyl-4-hydroxyphenyl)thio)hexanoate

생성물 1

HCID 40826DH 990

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

The ethyl 2-((3,5-di-tert-butyl-4-hydroxyphenyl)thio)hexanoate product (75 grams; 0.195 mole) obtained in Example 2 was dispersed in 300 ml. of 95% ethanol and 500 ml. of 5N potassium hydroxide added thereto. The resulting reaction mixture was heated on a steam bath at the boiling point under gentle reflux for about 90 minutes with occasional stirring. Following the heating period, the reaction mixture was poured into 2000 ml. of 5% HCl with vigorous stirring. The white precipitate formed upon acidification was obtained by filtration and washed with water. Recrystallization (twice) of the precipitate from a methylene chloride-hexane mixture gave the desired 2-((3,5-di-tert-butyl-4-hydroxyphenyl)thio)hexanoic acid compound having a melting point of 140°-142° C.

후처리

  1. additionwas dispersed in 300 ml
  2. customThe resulting reaction mixture
  3. temperaturewas heated on a steam bath at the boiling point
  4. temperatureunder gentle reflux for about 90 minutes with occasional stirring
  5. additionthe reaction mixture was poured into 2000 ml
  6. customThe white precipitate formed upon acidification
  7. customwas obtained by filtration
  8. washwashed with water
  9. customRecrystallization (twice) of the precipitate from a methylene chloride-hexane mixture

출처 및 근거

ORD 기록
ord-94e928ef751f4e1b8c9007a4846a1d4e
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012523

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