Potassium Iodide → 2,2-diethoxyethyl Benzoate

HRID 13677

반응식

HRID 13677 반응식
[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5]Cl)[CH3:2].[C:10]([O-:18])(=[O:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[K+].[I-].[K+].CN(C=O)C>C(OCC)(=O)C.O>[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

7

반응물 4

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 121282-Chloro-1,1-diethoxyethaneHCID 23661960Potassium Benzoate

생성물 1

HCID 118172582,2-diethoxyethyl Benzoate수율 84.8%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

Chloroacetaldehyde diethyl acetal (2.00 g), potassium benzoate (1.91 g), potassium iodide (0.41 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 then to Kugelrohr distillation at 110-120° C. and at 1 mmHg and thereby yielded the target compound (2.41 g) in a yield of 77%.

후처리

  1. temperatureby refluxing
  2. filtrationAfter filtration
  3. customthe organic layer was separated
  4. concentrationwas subjected to vacuum concentration
  5. distillationto Kugelrohr distillation at 110-120° C.

출처 및 근거

ORD 기록
ord-b38bb05c9a654ded9acc8930760c2a49
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728152B2

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