Ammonia → 2-(dimethoxymethyl)-5-methyl-4-(trifluoromethyl)-1H-imidazole

HRID 43467

반응식

HRID 43467 반응식
[CH2:1]1[C:6](=O)[N:5](Cl)C(=O)[CH2:2]1.[F:9][C:10]([F:21])([F:20])C(C1(C)SCCCS1)=O.[CH3:22][O:23][CH:24]([O:27][CH3:28])[CH:25]=O.[NH3:29]>C(#N)C.[N+]([O-])([O-])=O.[Ag+]>[CH3:22][O:23][CH:24]([O:27][CH3:28])[C:25]1[NH:29][C:1]([CH3:2])=[C:6]([C:10]([F:21])([F:20])[F:9])[N:5]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 31398ChlorosuccinimideHCID 162650Acetaldehyde, 2,2-dimethoxy-HCID 866484802,2,2-Trifluoro-1-(2-methyl-1,3-dithian-2-yl)ethanone

생성물 1

HCID 675492182-(dimethoxymethyl)-5-methyl-4-(trifluoromethyl)-1H-imidazole

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 6342Acetonitrile용매

실험 절차

NCS (870 mg, 6.51 mmol) and silver nitrate (1.48 g, 8.71 mmol) were dissolved in acetonitrile (40 mL) and distilled water (10 mL). 2,2,2-Trifluoro-1-(2-methyl-1,3-dithian-2-yl)ethanone obtained in Example (36a) (500 mg, 2.17 mmol) was added, and the mixture was stirred for 40 minutes. Thereafter, dimethoxyacetaldehyde (5.76 M aqueous solution, 0.4 mL, 23.0 mmol) and 28% aqueous ammonia (2 mL) were added, and the mixture was stirred at room temperature for 18 hours. The reaction solution was filtered through celite and then concentrated under reduced pressure. The resulting compound was used for the next reaction without purification.

후처리

  1. distillationdistilled water (10 mL)
  2. stirringthe mixture was stirred at room temperature for 18 hours
  3. filtrationThe reaction solution was filtered through celite
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting compound was used for the next reaction without purification

출처 및 근거

ORD 기록
ord-3540bec67c3547b392f9605095eb2780
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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