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Hydrochloric Acid → Benzenepropanoic acid, 3-(1,1-dimethylethyl)-4-hydroxy-, methyl ester

HRID 1461890
ノート
印刷プレビュー

反応式

HRID 1461890 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH2:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])[CH:8]=[C:9](C(C)(C)C)[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].Cl>C1(C)C=CC=CC=1>[C:1]([C:5]1[CH:6]=[C:7]([CH2:16][CH2:17][C:18]([O:20][CH3:21])=[O:19])[CH:8]=[CH:9][C:10]=1[OH:11])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 62603Methyl di-t-butyl hydroxyhydrocinnamate

生成物 1

HCID 3084638Benzenepropanoic acid, 3-(1,1-dimethylethyl)-4-hydroxy-, methyl ester収率 71.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 50 g of methyl 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, 2.5 g of conc. hydrochloric acid and 30 ml of toluene was refluxed for 2 hours while stirring. After the completion of the reaction, the reaction mixture was washed with water and the solvent wa distilled off. Hexane was added to the residue and the mixture was icecooled. The resulting crystals were collected by filtration and recrystallized from hexane to give 29 g of methyl 3-(3-tert-butyl-4-hydroxyphenyl)propionate as white crystals, m.p. 59°-61° C.

後処理

  1. temperaturewas refluxed for 2 hours
  2. customAfter the completion of the reaction
  3. washthe reaction mixture was washed with water
  4. distillationthe solvent wa distilled off
  5. additionHexane was added to the residue
  6. filtrationThe resulting crystals were collected by filtration
  7. customrecrystallized from hexane

出典と根拠

ORDレコード
ord-f941720abb724c46ac78a04023a1f2e3
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05077424

反応ノート

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