Ammonium Chloride → HCID 178515052, 화합물

HRID 596974노트

반응식

HRID 596974 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[C:7](=[O:17])[C:8]3[C:13]([S:14][C:15]=2[CH:16]=1)=[CH:12][CH:11]=[CH:10][CH:9]=3)#[N:2].[N-:18]=[N+:19]=[N-:20].[Na+].[Cl-].[NH4+]>CN(C)C=O>[NH:18]1[C:1]([C:3]2[CH:4]=[CH:5][C:6]3[C:7](=[O:17])[C:8]4[C:13]([S:14][C:15]=3[CH:16]=2)=[CH:12][CH:11]=[CH:10][CH:9]=4)=[N:2][N:20]=[N:19]1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 1039569-Oxo-9H-thioxanthene-3-carbonitrile

생성물 1

HCID 178515052HCID 178515052, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3-cyanothioxanthone (2.56 g), sodium azide (0.84 g) and ammonium chloride (0.70 g) in dimethylformamide (20 ml) was heated on a steam bath for 5 hrs. The nitrile dissolved after 2 hr., at the same time a precipitate of the product forming. Much solid crystallised out on cooling. The reaction mixture was poured into excess dilute hydrochloric acid, and the yellow precipitate was filtered off and washed with water. It was dissolved in dilute aqueous sodium hydroxide, filtered and reprecipitated with dilute hydrochloric acid. The product was filtered off and dried at 110° C, and then recrystallised from dimethylformamide and dried at 154° C/15mm. Hg, decomposes 290° C.

후처리

  1. temperaturewas heated on a steam bath for 5 hrs
  2. custom, at the same time a precipitate of the product forming
  3. customMuch solid crystallised out
  4. temperatureon cooling
  5. additionThe reaction mixture was poured into excess dilute hydrochloric acid
  6. filtrationthe yellow precipitate was filtered off
  7. washwashed with water
  8. dissolutionIt was dissolved in dilute aqueous sodium hydroxide
  9. filtrationfiltered
  10. customreprecipitated with dilute hydrochloric acid
  11. filtrationThe product was filtered off
  12. customdried at 110° C
  13. customrecrystallised from dimethylformamide
  14. customdried at 154° C/15mm. Hg
  15. customdecomposes 290° C.

출처 및 근거

ORD 기록
ord-d186bec9b9994d269f2b00423c35eb67
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012499

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