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Diethyl Oxalate → potassium (2Z)-3-cyano-1-ethoxy-1-oxobut-2-en-2-olate

HRID 1484681
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인쇄 미리보기

반응식

HRID 1484681 반응식
CC([O-])(C)C.[K+:6].C1OCCOCCOCCOCCOCCOC1.[C:25]([O:32][CH2:33][CH3:34])(=[O:31])[C:26]([O:28]CC)=O.[C:35](#[N:38])[CH2:36][CH3:37]>C1COCC1>[C:35](/[C:36](/[CH3:37])=[C:26](\[O-:28])/[C:25]([O:32][CH2:33][CH3:34])=[O:31])#[N:38].[K+:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7268Diethyl OxalateHCID 7854PropionitrileHCID 2855718-Crown-6HCID 23665647Potassium tert-butoxide

생성물 1

HCID 24824588potassium (2Z)-3-cyano-1-ethoxy-1-oxobut-2-en-2-olate수율 77.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

3.84 g potassium 2-methylpropan-2-olate (34.2 mmol, 1.0 eq.) and 723 mg 18-crown-6 (2.74 mmol, 0.08 eq.) were dissolved in THF and 5.00 g diethyl oxalate (34.2 mmol, 1.0 eq.) were added within 5 minutes. The reaction mixture was heated to 60° C. and 1.88 g propiononitrile (34.2 mm ol, 1.0 eq.) were added within 5 minutes. The reaction was stirred at 60° C. for 1 hour. The solid was filtered off, dried in vacuo at 50° C. to provide 5.11 g (26.4 mmol, 77%) of the crude product which was used without further purification.

후처리

  1. filtrationThe solid was filtered off
  2. customdried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-de2d867d9095487dac3e5ac4e8bcf3d5
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422268B2

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