Iodoethane → N-Ethyl-N-[3-(3-methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]propanamide

HRID 1906780ノート

反応式

HRID 1906780 の反応式
[CH3:1][C:2]1[N:6]2[N:7]=[C:8]([C:11]3[CH:12]=[C:13]([NH:17][C:18](=[O:21])[CH2:19][CH3:20])[CH:14]=[CH:15][CH:16]=3)[CH:9]=[CH:10][C:5]2=[N:4][N:3]=1.[H-].[Na+].[CH2:24](I)[CH3:25]>CN(C)C=O>[CH2:24]([N:17]([C:13]1[CH:14]=[CH:15][CH:16]=[C:11]([C:8]2[CH:9]=[CH:10][C:5]3[N:6]([C:2]([CH3:1])=[N:3][N:4]=3)[N:7]=2)[CH:12]=1)[C:18](=[O:21])[CH2:19][CH3:20])[CH3:25]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 7532416N-(3-(3-methyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)propionamide

生成物 1

HCID 15595647N-Ethyl-N-[3-(3-methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]propanamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 6.1 g of N-[3-(3-methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]propanamide in 200 ml of dry dimethylformamide under argon, was added 1.1 g of sodium hydride (50% in oil). The mixture was stirred for one hour, then 1.86 ml of ethyl iodide was added. This mixture was stirred overnight and then treated as described in Example 1. The chromatography fractions containing the product were combined and the solid recrystallized as described in Example 1, giving 4.37 g of the desired product, mp 145°-148° C.

後処理

  1. stirringThis mixture was stirred overnight
  2. additiontreated
  3. additionThe chromatography fractions containing the product
  4. customthe solid recrystallized

出典と根拠

ORDレコード
ord-6f33dd1c27134453b4f23de06535a6ec
出典データセット
uspto-grants-1987_03
特許番号
US04654343

反応ノート

読み込み中…