Pyridine → (3-tert-Butyl-isoxazol-5-yl)-carbamic acid 4-nitrophenyl ester

HRID 909234

反応式

HRID 909234 の反応式
[C:1]([C:5]1[CH:9]=[C:8]([NH2:10])[O:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].N1C=CC=CC=1.Cl[C:18]([O:20][C:21]1[CH:26]=[CH:25][C:24]([N+:27]([O-:29])=[O:28])=[CH:23][CH:22]=1)=[O:19]>ClCCl>[N+:27]([C:24]1[CH:23]=[CH:22][C:21]([O:20][C:18](=[O:19])[NH:10][C:8]2[O:7][N:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:9]=2)=[CH:26][CH:25]=1)([O-:29])=[O:28]

参加物

5

反応物 3

HCID 1049PyridineHCID 821294-Nitrophenyl chloroformateHCID 20956943-Tert-butyl-1,2-oxazol-5-amine

生成物 1

HCID 67408902(3-tert-Butyl-isoxazol-5-yl)-carbamic acid 4-nitrophenyl ester収率 41%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-tert-butyl-isoxazol-5-ylamine (2.50 g, 17.83 mmol) in dichloromethane was treated with pyridine (2 mL, 26.7 mmol) followed by p-nitrophenyl chloroformate (3.77 g, 18.73 mmol). The mixture was stirred at room temperature for 2 hours. The reaction mixture was washed with 1N HCl, filtered, and concentrated under reduced pressure. The residue was triturated with ether and collected by filtration to afford 2.2 g of product (41% yield).

後処理

  1. washThe reaction mixture was washed with 1N HCl
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was triturated with ether
  5. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-d9cc33f36e264b45ace5e5bb413f7dcb
出典データセット
uspto-grants-2011_09
特許番号
US08017641B2

関連ノート

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