Ammonium formate → 2,5-Bis(2-ethylhexyloxy)aniline

HRID 1050493

反応式

HRID 1050493 の反応式
[CH2:1]([CH:3]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH:14]([CH2:19][CH3:20])[CH2:15][CH2:16][CH2:17][CH3:18])=[CH:8][C:7]=1[N+:21]([O-])=O)[CH3:2].C([O-])=O.[NH4+]>CC(O)C>[CH2:1]([CH:3]([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH:14]([CH2:19][CH3:20])[CH2:15][CH2:16][CH2:17][CH3:18])=[CH:8][C:7]=1[NH2:21])[CH3:2]

参加物

4

反応物 2

HCID 2723923Ammonium formateHCID 896015891,4-Bis(2-ethylhexyloxy)-2-nitrobenzene

生成物 1

HCID 896017572,5-Bis(2-ethylhexyloxy)aniline

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

反応条件

温度
80 °C

実験手順

1,4-Bis(2-ethylhexyloxy)-2-nitrobenzene (11.4 g, 0.03 mol) is dissolved in 2-propanol (100 ml) and degassed under vacuum, purging to nitrogen. 10% (w/w) Pd/C (0.52 g) is added and the mixture heated to 80° C. Water (10 ml) is added, followed by solid ammonium formate (18.9 g, 0.3 mol). After a further 1 hour at 80° C., the reaction mixture is allowed to cool then filtered to remove catalyst, to give a colourless solution which darkened rapidly on standing. The material is used immediately as an isopropanol solution (quant.).

後処理

  1. customdegassed under vacuum
  2. custompurging to nitrogen
  3. addition10% (w/w) Pd/C (0.52 g) is added
  4. additionWater (10 ml) is added
  5. temperatureto cool
  6. filtrationthen filtered
  7. customto remove catalyst
  8. customto give a colourless solution which

出典と根拠

ORDレコード
ord-2417ed5c16a4427580aa39c33b5960f2
出典データセット
uspto-grants-2016_07
特許番号
US09383621B2

関連ノート

読み込み中…