Hydrochloric Acid → 4-(4-bromophenyl)-3-methyl-4,5-dihydro-1H-1,2,4-triazol-5-one

HRID 1484507

반응식

HRID 1484507 반응식
[C:1]([NH:4][NH:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([Br:15])=[CH:11][CH:10]=1)=[O:7])(=O)[CH3:2].[OH-].[Na+].Cl>O>[Br:15][C:12]1[CH:13]=[CH:14][C:9]([N:8]2[C:1]([CH3:2])=[N:4][NH:5][C:6]2=[O:7])=[CH:10][CH:11]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 232741832-acetyl-N-(4-bromophenyl)hydrazinecarboxamide

생성물 1

HCID 14877914-(4-bromophenyl)-3-methyl-4,5-dihydro-1H-1,2,4-triazol-5-one

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
130 °C

실험 절차

A large microwave tube was filled in with 2-acetyl-N-(4-bromophenyl)hydrazinecarboxamide (1.8 g, 6.62 mmol) and 2M aqueous NaOH (9 mL, 18 mmol). The reaction mixture was heated under microwave irradiation for 20 min at 130° C. Water (ca 18 mL) was added and the pH was adjusted to 4 by dropwise addition of aqueous HCl, with stirring. The thick precipitate was collected by filtration, washed with small amounts of cold water and dried. A small amount (220 mg) was purified by analytical preparation leading to 195 mg of the title compound.

후처리

  1. filtrationThe thick precipitate was collected by filtration
  2. washwashed with small amounts of cold water
  3. customdried
  4. customA small amount (220 mg) was purified by analytical preparation

출처 및 근거

ORD 기록
ord-ed06d3196331403db184342ecda5e251
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422252B2

연결된 노트

불러오는 중…