HCID 54321252, 화합물 → 3,4-Diamino-n-phenylbenzamide

HRID 1406434노트

반응식

HRID 1406434 반응식
[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]

참가 물질

5

반응물 2

HCID 54321252HCID 54321252, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 181854863,4-Diamino-n-phenylbenzamide

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-2628b98d87ea48b0bf80e4ed9d5488e0
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916599B2

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