Water → (2,4-Bis(1,1-dimethylpropyl)phenoxy)acetic acid

HRID 1756889노트

반응식

HRID 1756889 반응식
[C:1]([C:6]1[CH:18]=[C:17]([C:19]([CH2:22][CH3:23])([CH3:21])[CH3:20])[CH:16]=[CH:15][C:7]=1[O:8][CH2:9][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:18]=[C:17]([C:19]([CH2:22][CH3:23])([CH3:21])[CH3:20])[CH:16]=[CH:15][C:7]=1[O:8][CH2:9][C:10]([OH:12])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 19391876Ethyl [2,4-bis(2-methylbutan-2-yl)phenoxy]acetate

생성물 1

HCID 83411(2,4-Bis(1,1-dimethylpropyl)phenoxy)acetic acid수율 133.8%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

The above ethyl 2-(2,4-di-t-amylphenoxy)acetate (293 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 (289.5 g) was added thereto, followed by extraction. The water layer was separated with a separatory funnel, and the toluene layer was washed with water (289.5 g). Then, the toluene layer was concentrated by distillation under ordinary pressure for the recovery 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.

후처리

  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 (289.5 g)
  7. concentrationThen, the toluene layer was concentrated by distillation under ordinary pressure for the recovery of toluene, which

출처 및 근거

ORD 기록
ord-145f2852474d403f8ef98a103d0fb8c9
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05442114

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