Dimethylformamide → 2,2-diethoxyethyl Benzoate

HRID 13678

反応式

HRID 13678 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+].[Br-].[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 6228DimethylformamideHCID 121282-Chloro-1,1-diethoxyethaneHCID 253877Potassium BromideHCID 23661960Potassium Benzoate

生成物 1

HCID 118172582,2-diethoxyethyl Benzoate収率 34.1%

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 bromide (0.30 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 washed with water (30 mL) and was dried over anhydrous sodium sulfate. Subsequent filtration and vacuum concentration yielded the target compound (0.97 g) in a yield of 31%.

後処理

  1. temperatureby refluxing
  2. filtrationAfter filtration
  3. washthe organic layer was washed with water (30 mL)
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. filtrationSubsequent filtration and vacuum concentration

出典と根拠

ORDレコード
ord-50fe9b92db544c87abd868a71e54946d
出典データセット
uspto-grants-2010_06
特許番号
US07728152B2

関連ノート

読み込み中…