Methyl iodide → 6-Bromo-2-methylsulfanyl-3H-pyrrolo[2,1-f][1,2,4]triazin-4-one

HRID 1262278ノート

反応式

HRID 1262278 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[N:9]([CH:10]=1)[NH:8][C:7](=[S:11])[NH:6][C:5]2=[O:12].[CH3:13]I>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]2[N:9]([CH:10]=1)[N:8]=[C:7]([S:11][CH3:13])[NH:6][C:5]2=[O:12]

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 574161296-Bromo-2-sulfanylidene-2,3-dihydropyrrolo[2,1-f][1,2,4]triazin-4(1H)-one

生成物 1

HCID 1363603016-Bromo-2-methylsulfanyl-3H-pyrrolo[2,1-f][1,2,4]triazin-4-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

Into a round bottom flask, 6-Bromo-2-thioxo-2,3-dihydro-1H-pyrrolo[2,1-f][1,2,4]triazin-4-one (11.20 g, 0.04551 mol), Tetrahydrofuran (200 mL) and Methyl iodide (6.517 mL, 0.1047 mol) were added, respectively. The reaction was stirred at 45° C. for one hour. The solid was filtered. The solvent was removed under vacuum to give a solid. The combined solid was partitioned with water (500 mL) and saturated NaHCO3 (500 mL). The mixture was stirred for 30 minutes. The solid was filtered and washed with water to give 6-Bromo-2-methylsulfanyl-3H-pyrrolo[2,1-f][1,2,4]triazin-4-one as a white solid (5.80, 49%).

後処理

  1. filtrationThe solid was filtered
  2. customThe solvent was removed under vacuum
  3. customto give a solid
  4. customThe combined solid was partitioned with water (500 mL) and saturated NaHCO3 (500 mL)
  5. stirringThe mixture was stirred for 30 minutes
  6. filtrationThe solid was filtered
  7. washwashed with water

出典と根拠

ORDレコード
ord-c784874467094115b86f8cc95e451658
出典データセット
uspto-grants-2013_06
特許番号
US08471005B2

反応ノート

読み込み中…