Water → Butanoic acid, 2-(2,4-bis(1,1-dimethylpropyl)phenoxy)-

HRID 1756890ノート

反応式

HRID 1756890 の反応式
[C:1]([C:6]1[CH:20]=[C:19]([C:21]([CH2:24][CH3:25])([CH3:23])[CH3:22])[CH:18]=[CH:17][C:7]=1[O:8][CH:9]([CH2:15][CH3:16])[C:10]([O:12]CC)=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2].[OH-].[Na+].S(=O)(=O)(O)O.O>C1(C)C=CC=CC=1>[C:1]([C:6]1[CH:20]=[C:19]([C:21]([CH2:24][CH3:25])([CH3:22])[CH3:23])[CH:18]=[CH:17][C:7]=1[O:8][CH:9]([CH2:15][CH3:16])[C:10]([OH:12])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 19391871Ethyl 2-[2,4-bis(2-methylbutan-2-yl)phenoxy]butanoate

生成物 1

HCID 625983Butanoic acid, 2-(2,4-bis(1,1-dimethylpropyl)phenoxy)-収率 122.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

The above ethyl 2-(2,4-di-t-amylphenoxy)butyrate (317.9 g) and 27% aqueous sodium hydroxide (401.4 g) were placed in a 3-liter flask. The mixture was kept at 98° C. for 6 hours, and the hydrolysis reaction was completed. After completion of the reaction, the mixture was adjusted to pH 2 or lower by the addition of 40% aqueous sulfuric acid (349.9 g) and water (250 g), and toluene (317.9 g) was added thereto, followed by extraction. The water layer was separated with a separatory funnel, and the toluene layer was washed with water (317.9 g). Then, the toluene layer was concentrated by distillation under ordinary pressure for the removal of toluene, which afforded a concentrated solution (357.6 g) of the carboxylic acid compound in toluene. The analysis revealed that the concentrated solution contained the desired carboxylic acid compound in a yield of 99% on the basis of the raw material ester compound.

後処理

  1. customthe hydrolysis reaction
  2. customAfter completion of the reaction
  3. additionwas added
  4. extractionfollowed by extraction
  5. customThe water layer was separated with a separatory funnel
  6. washthe toluene layer was washed with water (317.9 g)
  7. concentrationThen, the toluene layer was concentrated by distillation under ordinary pressure for the removal of toluene, which

出典と根拠

ORDレコード
ord-fe65d43e86444eecaf8d708634fbde03
出典データセット
uspto-grants-1995_08
特許番号
US05442114

反応ノート

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