Tert-butyl 3-[(5-{[bis(3-methylbutyl)amino]carbonyl}-2-nitrophenyl)amino]propylcarbamate → Tert-butyl 3-[(2-amino-5-{[bis(3-methylbutyl)amino]carbonyl}phenyl)amino]propylcarbamate

HRID 1160989ノート

反応式

HRID 1160989 の反応式
[CH3:1][CH:2]([CH3:34])[CH2:3][CH2:4][N:5]([CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[C:6]([C:8]1[CH:9]=[CH:10][C:11]([N+:26]([O-])=O)=[C:12]([NH:14][CH2:15][CH2:16][CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH:13]=1)=[O:7]>C(OCC)(=O)C.C(O)C.[Pd]>[NH2:26][C:11]1[CH:10]=[CH:9][C:8]([C:6]([N:5]([CH2:29][CH2:30][CH:31]([CH3:33])[CH3:32])[CH2:4][CH2:3][CH:2]([CH3:34])[CH3:1])=[O:7])=[CH:13][C:12]=1[NH:14][CH2:15][CH2:16][CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22]

参加物

4

反応物 1

HCID 68789966Tert-butyl 3-[(5-{[bis(3-methylbutyl)amino]carbonyl}-2-nitrophenyl)amino]propylcarbamate

生成物 1

HCID 68792100Tert-butyl 3-[(2-amino-5-{[bis(3-methylbutyl)amino]carbonyl}phenyl)amino]propylcarbamate収率 89%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21584252Ethanol ethylacetate溶媒

反応条件

温度
20 °C

実験手順

Tert-butyl 3-[(5-{[bis(3-methylbutyl)amino]carbonyl}-2-nitrophenyl)amino]propylcarbamate (1.65 g) in solution in a mixture of ethyl acetate/ethanol 2:1 (130 ml), and 10% palladium on carbon (165 mg) are introduced into an autoclave. After stirring for 3 hours under a hydrogen atmosphere (3 bar) at a temperature of approximately 20° C., the catalyst is eliminated by filtration on celite and the filtrate is concentrated under reduced pressure at 40° C. in order to produce the expected compound in the form of an oil (1.35 g; 89% yield).

後処理

  1. additionare introduced into an autoclave
  2. filtrationthe catalyst is eliminated by filtration on celite
  3. concentrationthe filtrate is concentrated under reduced pressure at 40° C. in order

出典と根拠

ORDレコード
ord-b4723765122e4470b573e57d93760c35
出典データセット
uspto-grants-2010_10
特許番号
US07816539B2

反応ノート

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