Benzoic Acid → 2,2-diethoxyethyl Benzoate

HRID 13679

반응식

HRID 13679 반응식
[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5]Cl)[CH3:2].[C:10]([OH:18])(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.O.CN(C=O)C>[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][O:18][C:10](=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH3:2]

참가 물질

8

반응물 4

HCID 243Benzoic AcidHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 121282-Chloro-1,1-diethoxyethane

생성물 1

HCID 118172582,2-diethoxyethyl Benzoate수율 56%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Chloroacetaldehyde diethyl acetal (2.00 g), benzoic acid (2.16 g), potassium iodide (0.27 g), potassium carbonate (1.11 g) and DMF (20 mL) were placed in a three-neck flask, followed by refluxing. Twenty hours later, the reaction mixture was cooled to room temperature, and water (30 mL) and ethyl acetate (80 mL) were added thereto, followed by stirring. After filtration, the organic layer was separated, was subjected to vacuum concentration and thereby yielded the target compound (1.74 g) in a yield of 56%.

후처리

  1. temperatureby refluxing
  2. filtrationAfter filtration
  3. customthe organic layer was separated
  4. concentrationwas subjected to vacuum concentration

출처 및 근거

ORD 기록
ord-5ddedaa9d9e64079942ac7ae57726df1
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728152B2

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