Ammonium Chloride → HCID 178515052、化合物

HRID 867203ノート

反応式

HRID 867203 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178515052HCID 178515052、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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 hrs., 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./15 mm Hg, decomposes 290° C.

後処理

  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./15 mm Hg
  15. customdecomposes 290° C.

出典と根拠

ORDレコード
ord-c8112292ec3f4fbebb8939e53640a4d3
出典データセット
uspto-grants-1978_07
特許番号
US04103015

反応ノート

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