Water → 2,6-Dimethyl-4-[3-(methylamino)-4-nitrophenoxy]aniline

HRID 424862노트

반응식

HRID 424862 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([NH:8][CH3:9])[CH:7]=1.[NH2:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([OH:21])=[CH:16][C:15]=1[CH3:22].CC(C)([O-])C.[K+].O>CN(C)C(=O)C>[NH2:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([O:21][C:2]2[CH:3]=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([NH:8][CH3:9])[CH:7]=2)=[CH:16][C:15]=1[CH3:22]

참가 물질

6

반응물 4

HCID 962WaterHCID 765434-Amino-3,5-dimethylphenolHCID 2580415-chloro-N-methyl-2-nitroanilineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 667016652,6-Dimethyl-4-[3-(methylamino)-4-nitrophenoxy]aniline수율 80.7%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

To a solution of N-(5-chloro-2-nitrophenyl)-N-methylamine (4.0 g) in N,N-dimethylacetamide (56 ml) were added 4-amino-3,5-dimethylphenol (2.9 g) and potassium t-butoxide (2.9 g) with stirring under ice-cooling, and the resulting mixture was stirred at 75-80° C. for 1 hour. After stirring, water (74 ml) was added to the reaction mixture, and the resulting mixture was cooled gradually to room temperature. The crystals precipitated were collected by filtration and dried in vacuo to afford the title compound (4.9 g, yield: 80%) as a yellow crystalline solid.

후처리

  1. temperaturecooling
  2. stirringthe resulting mixture was stirred at 75-80° C. for 1 hour
  3. stirringAfter stirring
  4. customThe crystals precipitated
  5. filtrationwere collected by filtration
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-bed30020c5a2485d9e0d88bee89b5d54
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106079B2

반응 노트

불러오는 중…