Ammonium Hydroxide → 3-(5-tert-Butylpyridazin-3-yl)-4-hydroxy-1-methylimidazolidin-2-one

HRID 363988ノート

反応式

HRID 363988 の反応式
Cl[C:2]1[N:7]=[N:6][C:5]([N:8]2[CH:12]([OH:13])[CH2:11][N:10]([CH3:14])[C:9]2=[O:15])=[CH:4][C:3]=1[C:16]([CH3:19])([CH3:18])[CH3:17].[OH-].[NH4+].[H][H]>[Pd].C(O)C>[CH3:19][C:16]([C:3]1[CH:4]=[C:5]([N:8]2[CH:12]([OH:13])[CH2:11][N:10]([CH3:14])[C:9]2=[O:15])[N:6]=[N:7][CH:2]=1)([CH3:17])[CH3:18]

参加物

6

反応物 3

HCID 14923Ammonium HydroxideHCID 1759313-(5-tert-Butyl-6-chloropyridazin-3-yl)-4-hydroxy-1-methylimidazolidin-2-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 1637233-(5-tert-Butylpyridazin-3-yl)-4-hydroxy-1-methylimidazolidin-2-one収率 122.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of 2.0 g (0.00702 mole) of 3-[6-chloro-5-(1,1-dimethylethyl)-3-pyridazinyl]-4-hydroxy-1-methyl-2-imidazolidinone, 2.0 ml of concentrated ammonium hydroxide, 300 milligrams (mg) of 10% palladium on carbon, and 100 ml of 2B ethanol was placed on a Parr shaker apparatus at 50 pounds of hydrogen. After one hour, when the consumption of hydrogen exceeded the theoretical amount, the mixture was filtered and concentrated, giving 2.15 g of a white solid, which was partitioned between 400 ml of methylene chloride and 40 ml of water. The layers were separated and the organic layer was dried with magnesium sulfate.

後処理

  1. customwhen the consumption of hydrogen
  2. filtrationthe mixture was filtered
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-fb614abbd1fe4932bbe05fe870b19cd5
出典データセット
uspto-grants-1986_08
特許番号
US04604127

反応ノート

読み込み中…