Ethyl 2-(3-nitrobenzylidene)-3-oxobutanoate → Decyl ethyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

HRID 1731549노트

반응식

HRID 1731549 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:17]=[CH:18][CH:19]=1)[CH:7]=[C:8]([C:14]([CH3:16])=O)[C:9]([O:11][CH2:12][CH3:13])=[O:10])([O-:3])=[O:2].[NH2:20]/[C:21](/[CH3:36])=[CH:22]\[C:23]([O:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])=[O:24]>C(O)C>[CH3:36][C:21]1[NH:20][C:14]([CH3:16])=[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:7]([C:6]2[CH:17]=[CH:18][CH:19]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[C:22]=1[C:23]([O:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])=[O:24]

참가 물질

4

반응물 2

HCID 367507Ethyl 2-(3-nitrobenzylidene)-3-oxobutanoateHCID 86741101Decyl 3-aminocrotonate

생성물 1

HCID 13233215Decyl ethyl 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 263 g (1 mol) of ethyl 2-(3-nitrobenzylidene)acetoacetate and 241 g (1 mol) of decyl 3-aminocrotonate in 2.4 liters of absolute ethanol was heated to boiling under nitrogen for 18 hours. The mixture was then filtered hot and the filtrate was evaporated in vacuo to about one half of the volume. The concentrated solution was cooled in ice, producing a thick mass of crystals. This was filtered off with suction, recrystallized from ethanol and, after washing with 0.5 liters of n-hexane, was dried in a vacuum oven at 60° C.

후처리

  1. filtrationThe mixture was then filtered hot
  2. customthe filtrate was evaporated in vacuo to about one half of the volume
  3. temperatureThe concentrated solution was cooled in ice
  4. customproducing a thick mass of crystals
  5. filtrationThis was filtered off with suction
  6. customrecrystallized from ethanol
  7. washafter washing with 0.5 liters of n-hexane
  8. customwas dried in a vacuum oven at 60° C.

출처 및 근거

ORD 기록
ord-8e4b9292e3384b1f80ec65014ab370ea
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04622332

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