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

HRID 1484507

反応式

HRID 1484507 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ed06d3196331403db184342ecda5e251
出典データセット
uspto-grants-2016_08
特許番号
US09422252B2

関連ノート

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