Acetonitrile → 1,3,5-Triazin-2(1H)-one, 1-(2,6-dimethylphenyl)-4-(methylamino)-

HRID 28053

反応式

HRID 28053 の反応式
Cl.[CH3:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[N:10]1[CH:15]=[N:14][C:13]([NH:16][CH3:17])=[N:12][C:11]1=[O:18].C(#N)C>CN(C=O)C.CC(N(C)C)=O>[CH3:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([CH3:2])[C:4]=1[N:10]1[CH:15]=[N:14][C:13]([NH:16][CH3:17])=[N:12][C:11]1=[O:18]

参加物

4

反応物 2

HCID 6342AcetonitrileHCID 204573331-(2',6'-Dimethylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one hydrochloride

生成物 1

HCID 1008051,3,5-Triazin-2(1H)-one, 1-(2,6-dimethylphenyl)-4-(methylamino)-

試薬・触媒・溶媒 1

HCID 22628260N,N-dimethylformamide N,N-dimethylacetamide溶媒

反応条件

温度
105 °C

実験手順

About 200 mg. of 1-(2',6'-dimethylphenyl)-4-methylamino-1,2-dihydro-1,3,5-triazin-2-one hydrochloride is introduced into a gas chromatograph hypo vial and dissolved in 1 ml. of acetonitrile. To the solution is added 0.2 ml. of DMF DMA reagent. The vial is sealed with crimper and heated at 105° C. for 15 minutes in an oven. Seven vials are made. The contents of the vials are then put into a long-neck round bottom flask and evaporated to dryness by a flask evaporator. The solid mass is dissolved in a mixture of 30 ml. of CH Cl3 and 20 ml. of water and shaken vigorously in a 60 ml. separatory funnel. The aqueous layer is discarded and 20 ml. of water is added and shaken. The CH Cl3 layer is then taken off and about 10 g. of anhydrous Na2SO4 is added, the CH Cl3 solution is decanted into a flask and evaporated to dryness. The solid material is dissolved in pentanone- 2 (about 80 ml.) at 70° C. The solution is concentrated and crystallizes upon cooling. The crystals are collected and dried in a desiccator with P2O5 with vacuum for one hour.

後処理

  1. dissolutiondissolved in 1 ml
  2. additionTo the solution is added 0.2 ml
  3. customThe vial is sealed with crimper
  4. customThe contents of the vials are then put into a long-neck round bottom flask
  5. customevaporated to dryness by a flask
  6. customevaporator
  7. dissolutionThe solid mass is dissolved in a mixture of 30 ml
  8. additionof water is added
  9. stirringshaken
  10. additionof anhydrous Na2SO4 is added
  11. customthe CH Cl3 solution is decanted into a flask
  12. customevaporated to dryness
  13. dissolutionThe solid material is dissolved in pentanone- 2 (about 80 ml.) at 70° C
  14. concentrationThe solution is concentrated
  15. customcrystallizes
  16. temperatureupon cooling
  17. customThe crystals are collected
  18. dry with materialdried in a desiccator with P2O5 with vacuum for one hour

出典と根拠

ORDレコード
ord-bfa51a92eda74a3ebeec4cf63a4d7673
出典データセット
uspto-grants-1980_09
特許番号
US04225315

関連ノート

読み込み中…