HCID 54321252、化合物 → 3,4-Diamino-n-phenylbenzamide

HRID 1406434ノート

反応式

HRID 1406434 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:16]=[CH:17][C:18]=1[N+:19]([O-])=O)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:8])([O-])=O.[H][H]>C1COCC1.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([CH:16]=[CH:17][C:18]=1[NH2:19])[C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:8]

参加物

5

反応物 2

HCID 54321252HCID 54321252、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 181854863,4-Diamino-n-phenylbenzamide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of the product obtained at (1a) (19.0 g, 46.3 mmol) in 200 mL of THF was combined with 10% palladium on charcoal (3.0 g) and hydrogenated in a Parr apparatus at ambient temperature for 20 h at 3.5 bar hydrogen pressure. Then the mixture is filtered and the filtrate is concentrated i.vac. The residue is purified by chromatography on silica gel (eluent gradient: dichloromethane/(methanol/conc. ammonia=95:5)=100:0->92:8).

後処理

  1. additionA mixture of the product
  2. filtrationThen the mixture is filtered
  3. concentrationthe filtrate is concentrated i.vac
  4. customThe residue is purified by chromatography on silica gel (eluent gradient: dichloromethane/(methanol/conc. ammonia=95:5)=100:0->92:8)

出典と根拠

ORDレコード
ord-2628b98d87ea48b0bf80e4ed9d5488e0
出典データセット
uspto-grants-2014_12
特許番号
US08916599B2

反応ノート

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