Piperidine → 6-[(E)-2-(2-ethoxyphenyl)vinyl]-3-methyl-5-nitro-1-propyl-1H-pyrimidine-2,4-dione

HRID 496310

반응식

HRID 496310 반응식
[CH3:1][N:2]1[C:7](=[O:8])[C:6]([N+:9]([O-:11])=[O:10])=[C:5]([CH3:12])[N:4]([CH2:13][CH2:14][CH3:15])[C:3]1=[O:16].[CH2:17]([O:19][C:20]1[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=1[CH:22]=O)[CH3:18].N1CCCCC1>C(O)C>[CH2:17]([O:19][C:20]1[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=1/[CH:22]=[CH:12]/[C:5]1[N:4]([CH2:13][CH2:14][CH3:15])[C:3](=[O:16])[N:2]([CH3:1])[C:7](=[O:8])[C:6]=1[N+:9]([O-:11])=[O:10])[CH3:18]

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 11950Benzaldehyde, 2-ethoxy-HCID 223255723,6-dimethyl-5-nitro-1-propyl-1H-pyrimidine-2,4-dione

생성물 1

HCID 223255706-[(E)-2-(2-ethoxyphenyl)vinyl]-3-methyl-5-nitro-1-propyl-1H-pyrimidine-2,4-dione수율 75.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 3,6-dimethyl-5-nitro-1-propyl-1H-pyrimidine-2,4-dione (6.25 g, 27.5 mmol), 2-ethoxybenzaldehyde (4.24 mL, 30.3 mmol), piperidine (2.83 mL, 28.6 mmol) and 3 Å molecular sieves (8.75 g) in ethanol (125 mL) was refluxed for 5 hours. The resulting suspension was filtered and the filtrate was evaporated under reduced pressure. The residue was triturated with isopropyl ether and the precipitate collected by filtration and dried under vacuum to yield 6-[(E)-2-(2-ethoxyphenyl)vinyl]-3-methyl-5-nitro-1-propyl-1H-pyrimidine-2,4-dione (7.42 g, 75%) as a yellow solid.

후처리

  1. temperaturewas refluxed for 5 hours
  2. filtrationThe resulting suspension was filtered
  3. customthe filtrate was evaporated under reduced pressure
  4. customThe residue was triturated with isopropyl ether
  5. filtrationthe precipitate collected by filtration
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-ded9ff69bbb7454797577c9f12b2c426
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943253B2

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