1-Chloro-2-nitrobenzene → 5-methyl-N-(2-nitrophenyl)-2-furanmethanamine

HRID 620476

반응식

HRID 620476 반응식
[CH3:1][C:2]1[O:6][C:5]([CH2:7][NH2:8])=[CH:4][CH:3]=1.Cl[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[N+:16]([O-:18])=[O:17]>C(N(CC)CC)C>[CH3:1][C:2]1[O:6][C:5]([CH2:7][NH:8][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[N+:16]([O-:18])=[O:17])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 69451-Chloro-2-nitrobenzeneHCID 27246835-Methyl-2-furylmethylamine

생성물 1

HCID 141828815-methyl-N-(2-nitrophenyl)-2-furanmethanamine수율 89%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A mixture of 40 parts of 5-methyl-2-furanmethanamine, 46 parts of 1-chloro-2-nitrobenzene and 210 parts of N,N-diethylethanamine was stirred and refluxed for 2 days. The reaction mixture was evaporated, water was added and the product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was purified by filtration over silica gel using trichloromethane as eluent. The filtrate was evaporated, yielding 62 parts (89%) of 5-methyl-N-(2-nitrophenyl)-2-furanmethanamine as a residue (intermediate 2).

후처리

  1. temperaturerefluxed for 2 days
  2. customThe reaction mixture was evaporated
  3. additionwater was added
  4. extractionthe product was extracted with dichloromethane
  5. customThe extract was dried
  6. filtrationfiltered
  7. customevaporated
  8. filtrationThe residue was purified by filtration over silica gel
  9. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-1f8a7b6f4fd84874ac5a3ad0dff613a5
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04820822

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