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Hydrochloric Acid → Ethyl 2-(2-methoxyphenyl)acetoacetate

HRID 1003155
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인쇄 미리보기

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HRID 1003155 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11].[CH3:15][C:16](C)([O-:18])C.[Na+].C(OCC)(=O)C.Cl>C(OC(C)C)(C)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]([C:16]([CH3:15])=[O:18])[C:10]([O:12][CH2:13][CH3:14])=[O:11]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl Acetate2회HCID 80160Ethyl (2-methoxyphenyl)acetateHCID 23676156Sodium t-butoxide

생성물 1

HCID 22118306Ethyl 2-(2-methoxyphenyl)acetoacetate수율 60.2%

시약·촉매·용매 1

HCID 7914Diisopropyl Ether
용매

반응 조건

온도
70 °C

실험 절차

A mixture of ethyl 2-methoxyphenyiacetate (11.6 g), sodium tert-butoxide (12.7 g) and ethyl acetate (15.8 g) in diisopropylether was heated at 70° C. for 2.5 hours and stirred at room temperature overnight. Ethyl acetate and hydrochloric acid (2M) were added and the organic phase dried (magnesium sulphate) and evaporated. The residue was distilled in vacuo to give ethyl 2-(2-methoxyphenyl)acetoacetate as a liquid (8.5 g), NMR 1.15 and 1.13(t,3h), 1.8 and 2.2(s,3H), 3.75 and 3.85(s,3H), 4.1-4.3(2q,2H), 5.15(s,1H), 6.9-7.3(m,4H), 13.1(s,1H).

후처리

  1. dry with materialthe organic phase dried (magnesium sulphate)
  2. customevaporated
  3. distillationThe residue was distilled in vacuo

출처 및 근거

ORD 기록
ord-2c4291d4e9fe4beb95a2cc965c33b5fb
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06046135

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