Sodium → HCID 178507074、化合物

HRID 989564ノート

反応式

HRID 989564 の反応式
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[N:6][N:7]=1.[Na].[NH2:10][C:11]1[NH:15][N:14]=[N:13][N:12]=1>C(#N)C>[NH:12]1[C:11]([NH:10][C:2]2[N:3]=[N:4][C:5]([NH:10][C:11]3[NH:15][N:14]=[N:13][N:12]=3)=[N:6][N:7]=2)=[N:15][N:14]=[N:13]1

参加物

5

反応物 3

HCID 5360545SodiumHCID 136733773,6-Dichloro-1,2,4,5-tetrazineHCID 178509299HCID 178509299、化合物

生成物 1

HCID 178507074HCID 178507074、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 3,6-dichloro-1,2,4,5-tetrazine (1.51 g, 10 mmol) in acetonitrile (70 ml) was added the sodium salt of 5-amino-1H-tetrazole (2.14 g, 10 mmol). The mixture was refluxed for 24 hours then allowed to cool to room temperature. The suspension was centrifuged until the supernatant liquid was clear. The liquid was decanted and the brown solid washed successively with acetonitrile and water. With each wash the solid was separated from the solvent by centrifugation followed by decantation. The isolated crude yield was 1.5 g (60%), this material was recrystallized from DMSO/methanol yielding an orange brown powder mp 264° C. dec; 1H NMR (deuteriomethylsulfoxide) ∂ 12.5 (br s, 4H); 13C NMR (deuteriomethylsulfoxide) ∂ 151.74, 158.25; IR (KBr) 3421, 3000, 1615, 1436, 1127 cm−1. A gas pycnometer density of 1.76 g/cm3 was also determined and a drop height of 195 cm was measured (Type 12, HMX=24-27 cm).

後処理

  1. temperatureThe mixture was refluxed for 24 hours
  2. customThe liquid was decanted
  3. washthe brown solid washed successively with acetonitrile and water
  4. washWith each wash the solid
  5. customwas separated from the solvent by centrifugation
  6. customThe isolated crude yield was 1.5 g (60%), this material was recrystallized from DMSO/methanol yielding an orange brown powder mp 264° C. dec

出典と根拠

ORDレコード
ord-5e34ff6765e84dc6a752eb3949034ad5
出典データセット
uspto-grants-2002_10
特許番号
US06458227B1

反応ノート

読み込み中…