Potassium Carbonate → {2-[2-(Dimethylamino)-3-nitropyrrolyl]ethyl}[(6-chloro(3-pyridyl))methyl][(4-chlorophenyl)methyl]amine

HRID 549229ノート

反応式

HRID 549229 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]([CH2:18][CH2:19]Cl)[CH2:10][C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)=[CH:4][CH:3]=1.[CH3:21][N:22]([CH3:31])[C:23]1[NH:24][CH:25]=[CH:26][C:27]=1[N+:28]([O-:30])=[O:29].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:21][N:22]([CH3:31])[C:23]1[NH:24][CH:25]=[C:26]([CH2:19][CH2:18][N:9]([CH2:8][C:5]2[CH:6]=[N:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:10][C:11]2[CH:12]=[CH:13][C:14]([Cl:17])=[CH:15][CH:16]=2)[C:27]=1[N+:28]([O-:30])=[O:29]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 45121913N,N-Dimethyl-3-nitro-1H-pyrrol-2-amineHCID 86624870(6-Chloro(3-pyridyl)methyl](2-chloroethyl)[(4-chlorophenyl)methyl]amine

生成物 1

HCID 86624871{2-[2-(Dimethylamino)-3-nitropyrrolyl]ethyl}[(6-chloro(3-pyridyl))methyl][(4-chlorophenyl)methyl]amine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

This compound was prepared in a manner analogous to that set forth in Step G of Example 1, using 0.47 gram (0.0014 mole) of [(6-chloro(3-pyridyl)methyl](2-chloroethyl)[(4-chlorophenyl)methyl]amine (prepared in Steps A and B of the present Example), 0.2 gram (0.0013 mole) of dimethyl(3-nitropyrrol-2-yl)amine and 0.45 gram (0.0032 mole) of potassium carbonate in 20 mL of DMF. The crude product was purified with column chromatography on silica gel. Elution was accomplished using 50% hexane in diethyl as an eluant. The appropriate fractions were combined and concentrated under reduced pressure, yielding 0.05 gram of Compound 214. The NMR spectrum was consistent with the proposed structure.

後処理

  1. customThis compound was prepared in a manner analogous to that set forth in Step G of Example 1
  2. customThe crude product was purified with column chromatography on silica gel
  3. washElution
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e6894f8dcb064c0eaed8eda8d7f4875a
出典データセット
uspto-grants-2011_05
特許番号
US07943642B2

反応ノート

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