Dimethylformamide → 2-(Ethylthio)-1-methyl-4-nitro-1H-imidazole

HRID 653080ノート

反応式

HRID 653080 の反応式
[CH2:1]([SH:3])[CH3:2].CN(C)C=O.[OH-].[K+].[CH3:11][N:12]1[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[N:14]=[C:13]1S(C)(=O)=O>O>[CH3:11][N:12]1[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[N:14]=[C:13]1[S:3][CH2:1][CH3:2]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6343EthanethiolHCID 14797Potassium Hydroxide2 回HCID 3316921-Methyl-2-methylsulfonyl-4-nitroimidazole

生成物 1

HCID 139122322-(Ethylthio)-1-methyl-4-nitro-1H-imidazole収率 57.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Ethyl mercaptan (5.14 g, 0.083 mole) was added to dimethylformamide (140 ml) containing potassium hydroxide (4.6 g, 0.08 mole). This was stirred for 90 minutes until all the potassium hydroxide had dissolved. To this solution was added 1-methyl-2-methylsulfonyl-4-nitroimidazole (8.5 g, 0.04 mole) and the reaction stirred for 2 hours at room temperature. The reaction mixture was then added to water (500 ml) and stirred in an ice bath for an additional hour. The crystalline product was filtered off and dried to give 5.6 g of crude product. This was recrystallized from ethanol/water to give 4.3 g of product.

後処理

  1. dissolutionhad dissolved
  2. stirringstirred in an ice bath for an additional hour
  3. filtrationThe crystalline product was filtered off
  4. customdried
  5. customto give 5.6 g of crude product
  6. customThis was recrystallized from ethanol/water

出典と根拠

ORDレコード
ord-98dcc45122344eb9aa390776ddb84b53
出典データセット
uspto-grants-1987_06
特許番号
US04675337

反応ノート

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