Thiosemicarbazide → 5-(2-amino-6H-1,3,4-thiadiazin-5-yl)-3-nitropyrocatechol hydrobromide

HRID 274468

反応式

HRID 274468 の反応式
[Br:1][CH2:2][C:3]([C:5]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[C:8]([OH:14])=[C:7]([OH:15])[CH:6]=1)=O.[NH2:16][NH:17][C:18]([NH2:20])=[S:19]>C(O)CCC>[BrH:1].[NH2:20][C:18]1[S:19][CH2:2][C:3]([C:5]2[CH:6]=[C:7]([OH:15])[C:8]([OH:14])=[C:9]([N+:11]([O-:13])=[O:12])[CH:10]=2)=[N:16][N:17]=1

参加物

4

反応物 2

HCID 2723789ThiosemicarbazideHCID 218455962-Bromo-1-(3,4-dihydroxy-5-nitro-phenyl)-ethanone

生成物 1

HCID 1356653275-(2-amino-6H-1,3,4-thiadiazin-5-yl)-3-nitropyrocatechol hydrobromide

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A solution of 1.38 g of 2-bromo-3',4'-dihydroxy-5'-nitroacetophenone and 461 mg of thiosemicarbazide in 20 ml of n-butanol is heated to boiling under reflux for 60 minutes. After cooling to room temperature the crystals are filtered under suction and recrystallized from n-butanol. There is obtained 5-(2-amino-6H-1,3,4-thiadiazin-5-yl)-3-nitropyrocatechol hydrobromide of m.p. 265°-267°.

後処理

  1. temperatureunder reflux for 60 minutes
  2. filtrationare filtered under suction
  3. customrecrystallized from n-butanol

出典と根拠

ORDレコード
ord-2e434c7299e3461bb2b24c3e639093e1
出典データセット
uspto-grants-1995_02
特許番号
US05389653

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