Sodium Hydroxide → HCID 178518972, 화합물

HRID 1781618노트

반응식

HRID 1781618 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 178518972HCID 178518972, 화합물수율 94%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-836e3f9d0818470090395e9e815e5fd8
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05633387

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