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

HRID 424862ノート

反応式

HRID 424862 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bed30020c5a2485d9e0d88bee89b5d54
出典データセット
uspto-grants-2012_01
特許番号
US08106079B2

反応ノート

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