Sodium → HCID 178507074、化合物

HRID 431180ノート

反応式

HRID 431180 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(b,r s,4H); 13 C NMR (deuteriomethylsulfoxide) ∂ 151.74, 158.25; IR (KBr) 3421, 3000, 1615, 1436, 1127 cm−1.

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-4f91abb62ff44eaba6b96414fc3c6d58
出典データセット
uspto-grants-2003_12
特許番号
US06657059B2

反応ノート

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