Potassium Carbonate → HCID 67341951、化合物

HRID 1668667ノート

反応式

HRID 1668667 の反応式
[Cl:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[C:3]=1[CH2:4][NH:5][C:6]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[C:8](Cl)[N:7]=1.[C:21]([O:25][C:26]([N:28]1[CH2:32][CH2:31][C@@H:30]([CH2:33][NH2:34])[CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22].C(=O)([O-])[O-].[K+].[K+]>CC#N>[Cl:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([Cl:20])[C:3]=1[CH2:4][NH:5][C:6]1[N:7]=[C:8]([NH:34][CH2:33][C@@H:30]2[CH2:31][CH2:32][N:28]([C:26]([O:25][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:27])[CH2:29]2)[CH:9]=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 1514454tert-Butyl (3S)-3-(aminomethyl)pyrrolidine-1-carboxylateHCID 59705189n-(2,6-Dichlorobenzyl)-6-chloro-3-nitropyridin-2-amine

生成物 1

HCID 67341951HCID 67341951、化合物収率 27.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 16 (100 mg, 0.34 mmol), (S)-tert-Butyl-3-(aminomethyl)pyrrolidine-1-carboxylate (0.4 g, 2.0 mmol), potassium carbonate (56.4 mg, 0.41 mmol) in 10 mL MeCN was stirred at reflux for 2 hours. The solvent was removed by vacuum and the residue was purified by silica gel chromatography (MeOH:DCM=1:10) giving 17 [46 mg, 27% yield].

後処理

  1. temperatureat reflux for 2 hours
  2. customThe solvent was removed by vacuum
  3. customthe residue was purified by silica gel chromatography (MeOH:DCM=1:10)

出典と根拠

ORDレコード
ord-162a6e66d05144caa87ad93662f9af14
出典データセット
uspto-grants-2011_08
特許番号
US07989459B2

反応ノート

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