2-Aminopyridine → N-(5-pyrimidinylmethylene)-2-pyridinamine

HRID 341122

反応式

HRID 341122 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[N:8]1[CH:13]=[C:12]([CH:14]=O)[CH:11]=[N:10][CH:9]=1>C(Cl)(Cl)Cl>[N:8]1[CH:13]=[C:12]([CH:14]=[N:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=2)[CH:11]=[N:10][CH:9]=1

参加物

4

反応物 2

HCID 104392-AminopyridineHCID 2761034Pyrimidine-5-carboxaldehyde

生成物 1

HCID 68282155N-(5-pyrimidinylmethylene)-2-pyridinamine収率 99.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒3 回

実験手順

A solution of 2-aminopyridine (11.314 g, 120.3 mmole) and pyrimidine-5-carboxaldehyde (14.0 g, 129.6 mmole) in chloroform (300 mL) was stirred at room temperature for 15 minutes. The volatiles were then removed under reduced pressure (1 hour at 75° C.) to yield a yellow solid. The crude solid was dissolved in chloroform (300 mL), and the solution was stirred for 15 minutes. The volatiles were then removed under reduced pressure (1 hour at 75° C.) to yield a yellow solid. The crude solid was again dissolved in chloroform (300 mL), the solution was stirred for 15 minutes, and the volatiles were removed under reduced pressure (1 hour at 85° C.) to yield a yellow solid. This solid was dried in a vacuum oven overnight at 80° C. to yield 22.090 g (99.8%) of the title compound. 1H NMR (CDCl3) δ 9.26-9.32 (m, 4H), 8.52 (d, 1H), 7.82 (t, 1H), 7.42 (d, 1H), 7.26 (t, 1H).

後処理

  1. customThe volatiles were then removed under reduced pressure (1 hour at 75° C.)
  2. customto yield a yellow solid
  3. customThe volatiles were then removed under reduced pressure (1 hour at 75° C.)
  4. customto yield a yellow solid
  5. stirringthe solution was stirred for 15 minutes
  6. customthe volatiles were removed under reduced pressure (1 hour at 85° C.)
  7. customto yield a yellow solid
  8. customThis solid was dried in a vacuum oven overnight at 80° C.

出典と根拠

ORDレコード
ord-1cea720a338b4639ae73f96312819504
出典データセット
uspto-grants-2014_11
特許番号
US08895738B2

関連ノート

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