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

HRID 2231371

반응식

HRID 2231371 반응식
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]

참가 물질

5

반응물 3

HCID 177AcetaldehydeHCID 8082PiperidineHCID 69484Ethyl 4-chloroacetoacetate

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e34ba31881ce473ead9df2b0d6453007
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04782162

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