Dichloromethane → HCID 131715729, 화합물

HRID 868335노트

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HRID 868335 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[C:8]([CH2:12][CH3:13])[C:9]([OH:11])=[O:10])[CH:2]=1.[C:14]1([CH:20]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[N:21]2[CH2:26][CH2:25][N:24]([CH2:27][CH2:28][CH2:29][CH2:30][NH2:31])[CH2:23][CH2:22]2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.Cl.C(N=C=NCCCN(C)C)C.ClCCl.[C:53]([OH:60])(=[O:59])/[CH:54]=[CH:55]/[C:56]([OH:58])=[O:57]>C(O)C.C(OCC)C>[C:53]([OH:60])(=[O:59])/[CH:54]=[CH:55]/[C:56]([OH:58])=[O:57].[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[C:8]([CH2:12][CH3:13])[C:9]([NH:31][CH2:30][CH2:29][CH2:28][CH2:27][N:24]2[CH2:25][CH2:26][N:21]([CH:20]([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)[CH2:22][CH2:23]2)=[O:11])[CH:2]=1.[C:53]([OH:60])(=[O:59])/[CH:54]=[CH:55]/[C:56]([OH:58])=[O:57].[C:53]([OH:60])(=[O:59])/[CH:54]=[CH:55]/[C:56]([OH:58])=[O:57].[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[C:8]([CH2:12][CH3:13])[C:9]([NH:31][CH2:30][CH2:29][CH2:28][CH2:27][N:24]2[CH2:23][CH2:22][N:21]([CH:20]([C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:32]3[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=3)[CH2:26][CH2:25]2)=[O:10])[CH:2]=1

참가 물질

8

반응물 5

HCID 6344DichloromethaneHCID 444972Fumaric AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 139569931-(4-Aminobutyl)-4-(diphenylmethyl)piperazineHCID 539035433-(3-Pyridyl)-2-ethylacrylic acid

생성물 1

HCID 131715729HCID 131715729, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

A mixture of 0.8 g of 3-(3-pyridyl)-2-ethylacrylic acid, 2.2 g of 4-(4-diphenylmethyl-1-piperazinyl)butylamine, 0.87 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, and 30 ml of dichloromethane is stirred at room temperature overnight. The reaction mixture is washed with water and dried over magnesium sulfate, and the solvent is distilled off. The residue is chromatographed on silica gel with chloroform-methanol (30:1) to give a brown oil, which is dissolved in 5 ml of ethanol containing 1.0 g of fumaric acid. To the resulting solution is added 15 ml of diethyl ether, and the solid separated is collected to give 1.4 g of the title compound. m.p. 137°-141° C. (recrystallized from ethanol-diethyl ether)

후처리

  1. washThe reaction mixture is washed with water
  2. dry with materialdried over magnesium sulfate
  3. distillationthe solvent is distilled off
  4. customThe residue is chromatographed on silica gel with chloroform-methanol (30:1)
  5. customto give a brown oil, which
  6. customthe solid separated
  7. customis collected

출처 및 근거

ORD 기록
ord-09e7cd61eafe4904b53e2d065c232034
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778796

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