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N,2-Dimethyl-N-[2-nitro-5-(trifluoromethyl)phenyl]propanamide → 1-Methyl-2-(propan-2-yl)-6-(trifluoromethyl)-1H-benzimidazole

HRID 1288321
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반응식

HRID 1288321 반응식
[CH3:1][N:2]([C:16](=O)[CH:17]([CH3:19])[CH3:18])[C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[CH:5][C:4]=1[N+:13]([O-])=O>[Pd].C(O)C>[CH:17]([C:16]1[N:2]([CH3:1])[C:3]2[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[CH:5][C:4]=2[N:13]=1)([CH3:19])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 21504721N,2-Dimethyl-N-[2-nitro-5-(trifluoromethyl)phenyl]propanamide

생성물 1

HCID 215047021-Methyl-2-(propan-2-yl)-6-(trifluoromethyl)-1H-benzimidazole

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Shake 12.0 g. of N-methyl-2'-nitro-5'-trifluoromethylisobutyranilide in 100 ml. of ethanol containing 0.3 g. of 5% palladium on carbon at an initial pressure of approximately 50 lbs. per square inch. Filter, removing the solvent, and add 40 ml. of 4N hydrochloric acid and reflux for 30 minutes. Cool, and basify with sodium bicarbonate. Extract with ether and dry over sodium sulfate. Sublime at 55° C (0.1 mm) obtaining the product of this step.

후처리

  1. filtrationFilter
  2. customremoving the solvent
  3. additionadd 40 ml
  4. temperatureof 4N hydrochloric acid and reflux for 30 minutes
  5. temperatureCool
  6. extractionExtract with ether
  7. dry with materialdry over sodium sulfate
  8. customSublime at 55° C (0.1 mm) obtaining the product of this step

출처 및 근거

ORD 기록
ord-9962b0305907493783b4a1211cdd5ee5
출처 데이터셋
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03987182

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