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 → 5-amino-4-aminomethyl-1-(2-hydroxyethyl)-1H-pyrazole dihydrochloride

HRID 349578
ノート
印刷プレビュー

反応式

HRID 349578 の反応式
[NH2:1][C:2]1[N:6]([CH2:7][CH2:8][OH:9])[N:5]=[CH:4][C:3]=1[C:10]#[N:11].[ClH:12].O>CO.[Pd]>[ClH:12].[ClH:12].[NH2:1][C:2]1[N:6]([CH2:7][CH2:8][OH:9])[N:5]=[CH:4][C:3]=1[CH2:10][NH2:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 2198525-amino-1-(2-hydroxyethyl)-1H-pyrazole-4-carbonitrile

生成物 1

HCID 179619875-amino-4-aminomethyl-1-(2-hydroxyethyl)-1H-pyrazole dihydrochloride

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒2 回

実験手順

Under a nitrogen atmosphere, 10% palladium on active carbon (125 g) and methanol (3.75 L) were placed in a 5.0 L of three-necked flask. To the mixture was added 5-amino-4-cyano-1-(2-hydroxyethyl)-1H-pyrazole (250 g). The mixture was stirred at room temperature for 1 hour under a hydrogen atmosphere. To the reaction mixture was added 4N hydrogen chloride solution in methanol (1.65 L), and the mixture was stirred at room temperature for 1.5 hours under a hydrogen atmosphere. To the reaction mixture was added water (1.2 L). The catalyst was filtered off and washed with 50% aqueous methanol, and the filtrate was evaporated in vacuo. The residue was triturated with isopropanol/ethyl acetate (1:1). The precipitate was collected by filtration on a glass filter, washed with ethyl acetate and dried in vacuo to give 5-amino-4-aminomethyl-1-(2-hydroxyethyl)-1H-pyrazole dihydrochloride (358 g) as a white solid.

後処理

  1. stirringthe mixture was stirred at room temperature for 1.5 hours under a hydrogen atmosphere
  2. filtrationThe catalyst was filtered off
  3. washwashed with 50% aqueous methanol
  4. customthe filtrate was evaporated in vacuo
  5. customThe residue was triturated with isopropanol/ethyl acetate (1:1)
  6. filtrationThe precipitate was collected by filtration on a glass
  7. filtrationfilter
  8. washwashed with ethyl acetate
  9. customdried in vacuo

出典と根拠

ORDレコード
ord-26ece0ae1c69405497ec67ca65b0a995
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179801B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート