ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → 4-Amino-6-methyl-2,5-dihydro-1,2,4-triazin-3-one

HRID 265614
ノート
印刷プレビュー

反応式

HRID 265614 の反応式
C([NH:4][N:5]1[CH2:10][C:9]([CH3:11])=[N:8][NH:7][C:6]1=[O:12])(=O)C.Cl.O.[OH-].[Na+]>CO>[NH2:4][N:5]1[CH2:10][C:9]([CH3:11])=[N:8][NH:7][C:6]1=[O:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 11008343N-(6-Methyl-3-oxo-2,5-dihydro-1,2,4-triazin-4(3H)-yl)acetamide

生成物 1

HCID 109755004-Amino-6-methyl-2,5-dihydro-1,2,4-triazin-3-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
5 °C

実験手順

85 g of 4-acetylamino-6-methyl-3-oxo-2,3,4,5-tetrahydro-1,2,4-triazine in 250 ml of methanol are stirred together with 63 ml of hydrochloric acid (37%) for 4 hours at 50° C. After cooling to 5° C., 250 ml of icecold water and 125 ml of sodium hydroxide solution (50%) are added. The solvent is removed by evaporation in vacuo. The residue is taken up in 100 ml of ethanol, and the solvent is removed again in vacuo. The residue is taken up in 1200 ml of acetonitrile, undissolved salt precipitates are removed by filtration, the filtrate is concentrated to a small volume, the residue is caused to crystallize by adding 100 ml of acetic acid ethyl ester at 0° C., and the colorless crystals are filtered off and dried yielding 60.4 g (92% of the theoretical amount) of the title compound having a melting point of 118°-120° C.

後処理

  1. customThe solvent is removed by evaporation in vacuo
  2. customthe solvent is removed again in vacuo
  3. customundissolved salt precipitates
  4. customare removed by filtration
  5. concentrationthe filtrate is concentrated to a small volume
  6. customto crystallize
  7. additionby adding 100 ml of acetic acid ethyl ester at 0° C.
  8. filtrationthe colorless crystals are filtered off
  9. customdried

出典と根拠

ORDレコード
ord-464ee6fdfc0d4e258978e0470fbc8dd2
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05648487

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート