Benzoic Acid → 2,2-diethoxyethyl Benzoate

HRID 13679

反応式

HRID 13679 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 118172582,2-diethoxyethyl Benzoate収率 56%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-5ddedaa9d9e64079942ac7ae57726df1
出典データセット
uspto-grants-2010_06
特許番号
US07728152B2

関連ノート

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