Thiophosgene → ST50844634

HRID 849041ノート

反応式

HRID 849041 の反応式
[NH2:1][C:2]1[C:3]([CH3:9])=[N:4][N:5]([CH3:8])[C:6]=1[CH3:7].[C:10](Cl)(Cl)=[S:11]>C(Cl)(Cl)Cl.C([O-])(O)=O.[Na+]>[CH3:8][N:5]1[C:6]([CH3:7])=[C:2]([N:1]=[C:10]=[S:11])[C:3]([CH3:9])=[N:4]1

参加物

5

反応物 2

HCID 10040ThiophosgeneHCID 1616031,3,5-trimethyl-1H-pyrazol-4-amine

生成物 1

HCID 3263055ST50844634収率 101.5%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

A mixture of 4-amino-1,3,5-trimethylpyrazole (1.32 g, 10.6 mmol) in 50 mL each of CHCl3 and saturated aqueous NaHCO3 was treated dropwise with thiophosgene (0.812 mL, 10.6 mmol) and stirred vigorously for 20 minutes. The layers were separated and the organic phase was washed with brine. After drying (Na2SO4), the solvent was evaporated in vacuo to provide the title compound (1.8 g, brown oil) suitable for use directly in the next step.

後処理

  1. customThe layers were separated
  2. washthe organic phase was washed with brine
  3. dry with materialAfter drying (Na2SO4)
  4. customthe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-774bde4296584d1e9038dff9f6bcffbf
出典データセット
uspto-grants-2000_01
特許番号
US06011053

反応ノート

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