Potassium Iodide → 2,2-diethoxyethyl Benzoate

HRID 13677

反応式

HRID 13677 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 118172582,2-diethoxyethyl Benzoate収率 84.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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%.

後処理

  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.

出典と根拠

ORDレコード
ord-b38bb05c9a654ded9acc8930760c2a49
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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