Pyridine → Carbamic acid, 4-pyridinyl-, 4-nitrophenyl ester

HRID 445276ノート

反応式

HRID 445276 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.Cl[C:9]([O:11][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=1)=[O:10].N1C=CC=CC=1>C(Cl)Cl>[N:5]1[CH:6]=[CH:7][C:2]([NH:1][C:9](=[O:10])[O:11][C:12]2[CH:13]=[CH:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=2)=[CH:3][CH:4]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 17274-AminopyridineHCID 821294-Nitrophenyl chloroformate

生成物 1

HCID 10355188Carbamic acid, 4-pyridinyl-, 4-nitrophenyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-aminopyridine (1.97 g, 20.9 mmol) in DCM (75 mL) at 0° C. was added 4-nitrophenyl chloroformate (4.21 g, 20.9 mmol) and pyridine (1.7 mL, 20.9 mmol). Then, the mixture was stirred at RT overnight. The white precipitated was filtered off and washed with DCM (2×50 mL), and then dried in vacuo to give the title compound as a white solid, which was used in the next step without further purification. MS (ESI, positive ion) m/z: 260 (M+H).

後処理

  1. customThe white precipitated
  2. filtrationwas filtered off
  3. washwashed with DCM (2×50 mL)
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-016b120e0961490a95cef900c506ab88
出典データセット
uspto-grants-2013_07
特許番号
US08476297B2

反応ノート

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