N-methyl-N-(5-nitrobenzoxazol-2-ylmethyl)-4-nitrophenethylamine → N-methyl-N-(5-aminobenzoxazol-2-ylmethyl)-4-aminophenethylamine

HRID 345030

반응식

HRID 345030 반응식
[CH3:1][N:2]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([N+:24]([O-])=O)=[CH:20][CH:19]=1)[CH2:3][C:4]1[O:5][C:6]2[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][C:7]=2[N:8]=1>C(O)C.[Ni]>[CH3:1][N:2]([CH2:16][CH2:17][C:18]1[CH:19]=[CH:20][C:21]([NH2:24])=[CH:22][CH:23]=1)[CH2:3][C:4]1[O:5][C:6]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][C:7]=2[N:8]=1

참가 물질

4

반응물 1

HCID 19813428N-methyl-N-(5-nitrobenzoxazol-2-ylmethyl)-4-nitrophenethylamine

생성물 1

HCID 19813431N-methyl-N-(5-aminobenzoxazol-2-ylmethyl)-4-aminophenethylamine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

N-Methyl-N-(5-nitrobenzoxazol-2-ylmethyl)-4-nitrophenethyl-amine (0.78 g, 2.2 mmole) in ethanol (50 ml) containing Raney nickel (0.1 g) was stirred under a hydrogen atmosphere (50 psi =344.7 kPa) for 18 hours, by which time thin layer chromatographic analysis showed that all the starting material had been consumed [silica chromatography plates using methylene chloride/methanol (19:1) as the solvent]. The reaction mixture was then filtered and evaporated to give an oil which was azeotroped with toluene and triturated with ether. The decanted ether was evaporated to give the title compound as an oil, which was used directly without further purification, yield 0.45 g.

후처리

  1. customhad been consumed [silica chromatography plates
  2. filtrationThe reaction mixture was then filtered
  3. customevaporated
  4. customto give an oil which
  5. customwas azeotroped with toluene
  6. customtriturated with ether
  7. customThe decanted ether was evaporated

출처 및 근거

ORD 기록
ord-bef763eb70a0459698faf26f3e4eec1a
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055473

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