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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → 2-[(E)-3-(5-bromo-3-pyridinyl)-1-oxo-2-propenyl]-5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone

HRID 1612950
ノート
印刷プレビュー

反応式

HRID 1612950 の反応式
Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.[Br:24][C:25]1[CH:26]=[C:27]([CH:31]=[CH:32][C:33]([OH:35])=O)[CH:28]=[N:29][CH:30]=1.[CH:36]1([O:41][C:42]2[CH:43]=[C:44]([CH:50]3[N:54]([CH3:55])[NH:53][C:52](=[O:56])[CH2:51]3)[CH:45]=[CH:46][C:47]=2[O:48][CH3:49])[CH2:40][CH2:39][CH2:38][CH2:37]1>C(Cl)Cl>[Br:24][C:25]1[CH:26]=[C:27](/[CH:31]=[CH:32]/[C:33]([N:53]2[C:52](=[O:56])[CH2:51][CH:50]([C:44]3[CH:45]=[CH:46][C:47]([O:48][CH3:49])=[C:42]([O:41][CH:36]4[CH2:37][CH2:38][CH2:39][CH2:40]4)[CH:43]=3)[N:54]2[CH3:55])=[O:35])[CH:28]=[N:29][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27847353-(5-Bromopyridin-3-yl)prop-2-enoic acidHCID 27960291-Hydroxybenzotriazole hydrateHCID 197927655-[3-(Cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone

生成物 1

HCID 197773062-[(E)-3-(5-bromo-3-pyridinyl)-1-oxo-2-propenyl]-5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.20 mmol, 0.230 g), 1-hydroxybenzotriazole hydrate (1.20 mmol, 0.162 g) and 3-(5-bromo-3-pyridyl)propenoic acid (1.20 mmol, 0.274 g [see Nishikawa, et al, J Med Chem, 32, 583 (1989)] is suspended in dry methylene chloride (20 mL) at room temperature and stirred for 2 hours. To the suspension is added a solution of 5-[3(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone (1.20 mmol, 0.340 g) in dry methylene chloride (10 mL) and the resulting mixture is stirred at room temperature overnight followed by reflux for 24 hours. The homogenous solution is cooled to room temperature and the volatiles are removed in vacuo. The residue is partitioned between ethyl acetate (50 mL) and 1N NaOH (50 mL), the aqueous phase extracted with ethyl acetate (50 mL) and the combined organics are washed with water (50 mL) and dried (Na2SO4). Concentration in vacuo affords a white foam, which is purified via flash chromatography (SiO2 : concentration gradient ranging from 5% ethyl acetate/methylene chloride to 15% ethyl acetate/methylene chloride) to give the title compound as a white solid which is triturated with ether and hexane and dried in vacuo at 50° C. to provide analytically-pure material (0.52 mmol, 0.260 g, 52%). H-NMR (DMSO-d6, 400 MHz) δ8.82 (d, 1H, J=1.7 Hz); 8.66 (d, 1H, J=1.7 Hz); 8.41 (t, 1H); 7.71 (d, 2H, J=2.4 Hz,); 6.98 (d, 1H, J=1.5 Hz); 6.89 (m, 2H); 4.70 (m, 1H); 4.47 (dd, 1H, J=0.6, 1.7 Hz); 3.70 (s, 3H); 3.65 (m, 1H); 2.84 (s, 3H); 2.77 (m, 1H); 1.80 (m, 2H); 1.62 (m, 4H); 1.49 (m, 2H). IR (KBr, cm-1) 3460, 2940, 2860, 1748, 1660, 1623, 1515, 1445, 1435, 1425, 1326, 1260, 1235, 1208, 1150, 1130, 1015, 990, 962, 848, 680.

後処理

  1. stirringthe resulting mixture is stirred at room temperature overnight
  2. temperatureby reflux for 24 hours
  3. customthe volatiles are removed in vacuo
  4. customThe residue is partitioned between ethyl acetate (50 mL) and 1N NaOH (50 mL)
  5. extractionthe aqueous phase extracted with ethyl acetate (50 mL)
  6. washthe combined organics are washed with water (50 mL)
  7. dry with materialdried (Na2SO4)
  8. concentrationConcentration in vacuo
  9. customaffords a white foam, which
  10. customis purified via flash chromatography (SiO2 : concentration gradient ranging from 5% ethyl acetate/methylene chloride to 15% ethyl acetate/methylene chloride)

出典と根拠

ORDレコード
ord-d48ad8b108bb475880d53552594c0ca8
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05191084

反応ノート

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