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

HRID 653080노트

반응식

HRID 653080 반응식
[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]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6343EthanethiolHCID 14797Potassium Hydroxide2회HCID 3316921-Methyl-2-methylsulfonyl-4-nitroimidazole

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98dcc45122344eb9aa390776ddb84b53
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675337

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