Hydrochloric Acid → 3,5-Diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol

HRID 369687노트

반응식

HRID 369687 반응식
[CH2:1]([C:3]1[CH:4]=[C:5]([O:25]C(=O)C2C=CC=CC=2)[CH:6]=[C:7]([CH2:23][CH3:24])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][CH:16]([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[CH3:2].[OH-].[K+].Cl>CO.O>[CH2:23]([C:7]1[CH:6]=[C:5]([OH:25])[CH:4]=[C:3]([CH2:1][CH3:2])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][CH:16]([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[CH3:24]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 184296493,5-Diethyl-1-benzoyloxy-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene

생성물 1

HCID 184295323,5-Diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol수율 94%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 31.0 g of 3,5-diethyl-1-benzoyloxy-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene dissolved in 100 ml of methanol added a solution of 5.1 g of potassium hydroxide dissolved in 25 g of water. After stirring at room temperature for 1 hour, the reaction mixture was acidified by the addition of diluted hydrochloric acid and then concentrated. Water was added to the residue, which was extracted twice with ethyl acetate. The ethyl acetate layers were combined, washed with water, dried over magnesium sulfate and then concentrated. The residue was subjected to silica gel chromatography, which afforded 0.60 g of 3,5-diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol (yield, 94%), nD25.0 1.4890.

후처리

  1. concentrationconcentrated
  2. additionWater was added to the residue, which
  3. extractionwas extracted twice with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7f4f8b37ba5f4b04aeeca82ffbfaecc0
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06140274

반응 노트

불러오는 중…