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Formaldehyde → HCID 23300006, 화합물

HRID 1952750
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HRID 1952750 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.[CH2:15]=O.[CH3:17][CH:18]1[C:22](=[O:23])[NH:21][C:20]([C:24]2[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=2)=[N:19]1>>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:17][C:18]2([CH3:15])[C:22](=[O:23])[NH:21][C:20]([C:24]3[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=3)=[N:19]2)[CH2:11][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 712FormaldehydeHCID 13461-(2-Methoxyphenyl)piperazineHCID 23299969HCID 23299969, 화합물

생성물 1

HCID 23300006HCID 23300006, 화합물

실험 절차

A mixture of 1-(2-methoxyphenyl)piperazine (1.65 g) and 37-40% aqueous formaldehyde solution (0.39 ml) was stirred at ambient temperature under nitrogen for 10 minutes, then a suspension of 4-methyl-2-(3-pyridyl)-2-imidazolin-5-one (1.5 g) in industrial methylated spirit (75 ml) was added in one portion. The mixture was stirred and heated under reflux for 52 hours, then the solvent was removed in vacuo. The residue was triturated with a 49:49:2 mixture of ether, ethyl acetate and propan-2-ol, and the resulting solid was collected by filtration, washed with ethyl acetate, and dried in vacuo at ambient temperature to give 4-[4-(2-methoxyphenyl)piperazin-1-ylmethyl]-4-methyl-2-(3-pyridyl)-2-imidazolin-5-one as an off-white solid (1.55 g), m.p. 159-162° C.

후처리

  1. additionwas added in one portion
  2. stirringThe mixture was stirred
  3. temperatureheated
  4. temperatureunder reflux for 52 hours
  5. customthe solvent was removed in vacuo
  6. customThe residue was triturated with a 49:49:2 mixture of ether, ethyl acetate and propan-2-ol
  7. filtrationthe resulting solid was collected by filtration
  8. washwashed with ethyl acetate
  9. customdried in vacuo at ambient temperature

출처 및 근거

ORD 기록
ord-c7f1285b04434151b42841b4608e89b3
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06114334

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