Hydrochloric Acid → DH 990

HRID 596988

反応式

HRID 596988 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 40826DH 990

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94e928ef751f4e1b8c9007a4846a1d4e
出典データセット
uspto-grants-1977_03
特許番号
US04012523

関連ノート

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