Acetaldehyde → Ethyl 2-ethylidene-4-chloro-3-oxobutyrate

HRID 2231371

反応式

HRID 2231371 の反応式
N1CCC[CH2:3][CH2:2]1.[Cl:7][CH2:8][C:9](=[O:16])[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12].C(=O)C>C(OCC)(=O)C>[CH:2](=[C:10]([C:9](=[O:16])[CH2:8][Cl:7])[C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH3:3]

参加物

5

反応物 3

HCID 177AcetaldehydeHCID 8082PiperidineHCID 69484Ethyl 4-chloroacetoacetate

生成物 1

HCID 54518096Ethyl 2-ethylidene-4-chloro-3-oxobutyrate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

0.25 part by weight of piperidine is added dropwise to a mixture of 32.9 parts by weight of ethyl 4-chloroacetoacetate and 9.6 parts by weight of acetaldehyde at -20° C. The mixture is left to stand at -20° C. for 5 to 6 hours and ice-cold 1N hydrochloric acid and ethyl acetate are then added. The ethyl acetate phase is separated off, extracted twice more with 1N hydrochloric acid and then once with water, dried over magnesium sulphate and concentrated. 35.6 parts by weight of a yellow oil are obtained, and are distilled using a bulb tube (oven temperature 80° to 110° C. under 0.07 mm). 15.5 parts by weight of product are obtained.

後処理

  1. waitThe mixture is left
  2. customThe ethyl acetate phase is separated off
  3. extractionextracted twice more with 1N hydrochloric acid
  4. dry with materialonce with water, dried over magnesium sulphate
  5. concentrationconcentrated
  6. custom35.6 parts by weight of a yellow oil are obtained
  7. distillationare distilled
  8. custom(oven temperature 80° to 110° C. under 0.07 mm)
  9. custom15.5 parts by weight of product are obtained

出典と根拠

ORDレコード
ord-e34ba31881ce473ead9df2b0d6453007
出典データセット
uspto-grants-1988_11
特許番号
US04782162

関連ノート

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