Sodium Hydroxide → HCID 178518972、化合物

HRID 1781618ノート

反応式

HRID 1781618 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].[OH-:5].[Na+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[N+:14]#[C-:15]>O.CC(C)=O>[CH:11]1[CH:10]=[C:9]([N:14]2[NH:3][N:2]=[N:1][C:15]2=[O:5])[C:8]([Cl:7])=[CH:13][CH:12]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 27578001-Chloro-2-isocyanobenzene

生成物 1

HCID 178518972HCID 178518972、化合物収率 94%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒2 回

反応条件

温度
50 °C

実験手順

To sodium azide (0.65 g) dissolved in water (3.5 ml) a solution of 2-chlorophenylisocyanide, dichloride (2.09 g) in acetone (8 ml) was added with stirring. The mixture was heated to 50° C. and stirred for 15 minutes while maintaining this temperature. Thereafter, the mixture was heated for further 30 minutes with refluxing. An aqueous sodium hydroxide solution (about 40%, 2.5 g) and water (5 ml) were added thereto and the mixture was heated for 5 hours under stirring. After completing the reaction, the organic solvent was distilled off under reduced pressure and the water layer was washed once with toluene (5 ml). The mixture was adjusted to a pH of 1 with hydrochloric acid and the precipitate was collected by filtration with suction. The precipitate was washed with water followed-by drying to obtain light tan crystals 1-(2-chlorophenyl)-5(4H)-tetrazolinone (yield: 94%). melting point: 122°-124° C.

後処理

  1. additionwas added
  2. stirringstirred for 15 minutes
  3. temperaturewhile maintaining this temperature
  4. temperatureThereafter, the mixture was heated for further 30 minutes
  5. temperaturewith refluxing
  6. temperaturethe mixture was heated for 5 hours
  7. stirringunder stirring
  8. customthe reaction
  9. distillationthe organic solvent was distilled off under reduced pressure
  10. washthe water layer was washed once with toluene (5 ml)
  11. filtrationthe precipitate was collected by filtration with suction
  12. washThe precipitate was washed with water
  13. customfollowed-by drying

出典と根拠

ORDレコード
ord-836e3f9d0818470090395e9e815e5fd8
出典データセット
uspto-grants-1997_05
特許番号
US05633387

反応ノート

読み込み中…