HCID 23125017、化合物 → HCID 23125005、化合物

HRID 2223365ノート

反応式

HRID 2223365 の反応式
[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]

参加物

4

反応物 1

HCID 23125017HCID 23125017、化合物

生成物 1

HCID 23125005HCID 23125005、化合物収率 78.1%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8028Tetrahydrofuran溶媒

実験手順

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]+

後処理

  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)

出典と根拠

ORDレコード
ord-ff84efa0aa3b4308891ee84b171c5d8a
出典データセット
uspto-grants-2008_05
特許番号
US07375119B2

反応ノート

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