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

HRID 341122노트

반응식

HRID 341122 반응식
[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

참가 물질

4

반응물 2

HCID 104392-AminopyridineHCID 2761034Pyrimidine-5-carboxaldehyde

생성물 1

HCID 68282155N-(5-pyrimidinylmethylene)-2-pyridinamine수율 99.8%

시약·촉매·용매 1

HCID 6212Chloroform용매3회

실험 절차

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).

후처리

  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.

출처 및 근거

ORD 기록
ord-1cea720a338b4639ae73f96312819504
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895738B2

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