HCID 23125017, 화합물 → HCID 23125005, 화합물

HRID 2223365노트

반응식

HRID 2223365 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[CH:23]=[CH:22][C:14]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])=[CH:13][C:12]=2[N+:24]([O-])=O)=[O:10])=[N:6][CH:7]=1>O1CCCC1.[Ni]>[NH2:24][C:12]1[CH:13]=[C:14]([CH:22]=[CH:23][C:11]=1[C:9]([NH:8][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][N:6]=1)=[O:10])[C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16]

참가 물질

4

반응물 1

HCID 23125017HCID 23125017, 화합물

생성물 1

HCID 23125005HCID 23125005, 화합물수율 78.1%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매

실험 절차

t-Butyl 4-{[(5-chloropyridin-2-yl)amino]-carbonyl}-3-nitrobenzoate (3.2 g) obtained in Example 2(1) is dissolved in tetrahydrofuran (50 ml) and thereto is added Raney nickel, and the mixture is stirred at room temperature under hydrogen pressure (3 atm.) overnight. The insoluble materials are removed by filtration on Celite and the filtrate is concentrated under reduced pressure. The residue is purified by silica gel column chromatography (eluent: chloroform/ethyl acetate=20/1) to give t-butyl 3-amino-4-{[(5-chloropyridin-2-yl)amino]carbonyl}benzoate (2.3 g). APCI-MS M/Z: 348[M+H]+

후처리

  1. customThe insoluble materials are removed by filtration on Celite
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. customThe residue is purified by silica gel column chromatography (eluent: chloroform/ethyl acetate=20/1)

출처 및 근거

ORD 기록
ord-ff84efa0aa3b4308891ee84b171c5d8a
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07375119B2

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