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

HRID 620476

反応式

HRID 620476 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 141828815-methyl-N-(2-nitrophenyl)-2-furanmethanamine収率 89%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1f8a7b6f4fd84874ac5a3ad0dff613a5
出典データセット
uspto-grants-1989_04
特許番号
US04820822

関連ノート

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