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Ethyl 5-aminocarbonyl-4,6-diethoxy-2-(trifluoromethyl)-3-pyridinecarboxylate → Ethyl 5-cyano-4,6-diethoxy-2-(trifluoromethyl)-3-pyridinecarboxylate

HRID 1251956
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반응식

HRID 1251956 반응식
[NH2:1][C:2]([C:4]1[C:5]([O:22][CH2:23][CH3:24])=[C:6]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:7]([C:13]([F:16])([F:15])[F:14])=[N:8][C:9]=1[O:10][CH2:11][CH3:12])=O>O=P(Cl)(Cl)Cl>[C:2]([C:4]1[C:5]([O:22][CH2:23][CH3:24])=[C:6]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:7]([C:13]([F:16])([F:14])[F:15])=[N:8][C:9]=1[O:10][CH2:11][CH3:12])#[N:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 13726805Ethyl 5-aminocarbonyl-4,6-diethoxy-2-(trifluoromethyl)-3-pyridinecarboxylate

생성물 1

HCID 13726806Ethyl 5-cyano-4,6-diethoxy-2-(trifluoromethyl)-3-pyridinecarboxylate수율 24.6%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A mixture of 6.17 g (0.018 mol) of product of Example 23 and 100 ml of POCl3 was held at reflux for 7 hours and concentrated in vacuo. The residue was poured into water and extracted with ether. The ether extract was washed with 15% K2CO3, dried (MgSO4) and concentrated to give 1.44 g (24.6%) of product as an oil; nD25 1.4677.

후처리

temperature
at reflux for 7 hours
  • concentrationconcentrated in vacuo
  • additionThe residue was poured into water
  • extractionextracted with ether
  • extractionThe ether extract
  • washwas washed with 15% K2CO3
  • dry with materialdried (MgSO4)
  • concentrationconcentrated
  • 출처 및 근거

    ORD 기록
    ord-b6862867221b4da1addd3949b37f58f4
    출처 데이터셋
    uspto-grants-1988_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04741766

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