Chloropyrazine → HCID 57227784, 화합물

HRID 2260805

반응식

HRID 2260805 반응식
[CH3:1][N:2]1[CH2:7][C@@H:6]2[CH2:8][C@H:3]1[CH2:4][NH:5]2.Cl[C:10]1[CH:15]=[N:14][CH:13]=[CH:12][N:11]=1>C(Cl)Cl>[CH3:1][N:2]1[CH2:7][C@@H:6]2[CH2:8][C@H:3]1[CH2:4][N:5]2[C:10]1[CH:15]=[N:14][CH:13]=[CH:12][N:11]=1

참가 물질

4

반응물 2

HCID 73277ChloropyrazineHCID 11029795(1S,4S)-2-Methyl-2,5-diazabicyclo[2.2.1]heptane

생성물 1

HCID 57227784HCID 57227784, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
80 °C

실험 절차

A solution of 2.1 g of (S,S)-2-methyl-2,5-diazabicyclo[2.2.1]heptane prepared by the procedure of U. Jordis et al, Synthesis, 1990, 925, and 1.8 ml of 2-chloropyrazine in 8 ml of diazabicyclo[3.6.0]undecene-5 is heated to approximately 80° C. for 2 hours. The reaction solution is cooled, diluted with 100 ml of methylene chloride and washed with 30 ml of 5N aqueous sodium hydroxide. The organic layer is dried and concentrated in vacuo to dryness. The residue is purified by chromatography (aluminum oxide, Activity Grade 2.5; methylene chloride to 5% methyl alcohol/methylene chloride) to give 2.1 g of the desired product as a pale yellow oil:

후처리

  1. temperatureThe reaction solution is cooled
  2. washwashed with 30 ml of 5N aqueous sodium hydroxide
  3. customThe organic layer is dried
  4. concentrationconcentrated in vacuo to dryness
  5. customThe residue is purified by chromatography (aluminum oxide, Activity Grade 2.5; methylene chloride to 5% methyl alcohol/methylene chloride)

출처 및 근거

ORD 기록
ord-19199d6472b0477a9985a98b6cfa98b2
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05478939

연결된 노트

불러오는 중…