Dichloromethane → HCID 131715729、化合物

HRID 868335ノート

反応式

HRID 868335 の反応式
[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

参加物

8

反応物 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

生成物 1

HCID 131715729HCID 131715729、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-09e7cd61eafe4904b53e2d065c232034
出典データセット
uspto-grants-1988_10
特許番号
US04778796

反応ノート

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