Triethylamine → HCID 86632924、化合物

HRID 1628584ノート

反応式

HRID 1628584 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][NH:5][C:6](=[O:12])[O:7][C:8]([CH3:11])([CH3:10])[CH3:9].Cl[C:14]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][CH:17]=[CH:16][C:15]=1[N+:23]([O-:25])=[O:24].C(N(CC)CC)C>O1CCCC1.C(OCC)(=O)C>[N+:20]([C:19]1[CH:18]=[CH:17][CH:16]=[C:15]([N+:23]([O-:25])=[O:24])[C:14]=1[NH:1][CH2:2][CH2:3][CH2:4][NH:5][C:6](=[O:12])[O:7][C:8]([CH3:9])([CH3:11])[CH3:10])([O-:22])=[O:21]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 118141-Chloro-2,6-dinitrobenzeneHCID 2735700tert-Butyl (3-aminopropyl)carbamate

生成物 1

HCID 86632924HCID 86632924、化合物収率 99.5%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of tert-butyl (3-aminopropyl)carbamate (4.20 g, 24.1 mmol), 2-chloro-1,3-dinitrobenzene (4.07 g, 20.1 mmol) and triethylamine (5.60 mL, 40.2 mmol) in tetrahydrofuran (200 mL) was stirred at room temperature for 3 h. The reaction mixture was diluted with ethyl acetate, washed with water and brine, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with a 30% ethyl acetate/n-hexane mixture to give a yellow solid (6.79 g, 20.0 mmol, 99.5%).

後処理

  1. washwashed with water and brine
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel eluting with a 30% ethyl acetate/n-hexane mixture

出典と根拠

ORDレコード
ord-e27f12175eea4edfa302a50f45453219
出典データセット
uspto-grants-2014_07
特許番号
US08785460B2

反応ノート

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