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

HRID 274468

반응식

HRID 274468 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-2e434c7299e3461bb2b24c3e639093e1
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389653

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