Hydrogen Bromide → HCID 23149812、化合物

HRID 1670737

反応式

HRID 1670737 の反応式
N[C:2]1[C:3]([N+:13]([O-:15])=[O:14])=[CH:4][C:5]([Cl:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[BrH:16].N([O-])=O.[Na+].[OH-].[Na+]>O>[Br:16][C:2]1[C:3]([N+:13]([O-:15])=[O:14])=[CH:4][C:5]([Cl:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1

参加物

6

反応物 4

HCID 260Hydrogen BromideHCID 14798Sodium HydroxideHCID 27376454-Chloro-2-nitro-5-(trifluoromethyl)anilineHCID 23668193Sodium Nitrite

生成物 1

HCID 23149812HCID 23149812、化合物収率 56%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 5-amino-2-chloro-4-nitrobenzotrifluoride (synthesized according to the method described in J. Org. Chem., 60, 18, 1995, 5838-5842, 24.9 g) and 48% aqueous hydrogen bromide (400 ml) was ice-cooled. Sodium nitrite (12.9 g) was dissolved in a small amount of water and added dropwise thereto. The reaction mixture was stirred for 4 hr while warming from −5° C. to 15° C., ice-cooled and alkalified with a 6N aqueous sodium hydroxide solution. The precipitated solid was collected by filtration and washed with water to give a brown solid. The solid was purified by silica gel column chromatography (elution solvent:ethyl acetate-hexane (1:50)) to give 5-bromo-2-chloro-4-nitrobenzotrifluoride (17.7 g, yield 56%).

後処理

  1. customsynthesized
  2. temperaturecooled
  3. additionadded dropwise
  4. temperaturewhile warming from −5° C. to 15° C.
  5. temperatureice-cooled
  6. filtrationThe precipitated solid was collected by filtration
  7. washwashed with water
  8. customto give a brown solid
  9. customThe solid was purified by silica gel column chromatography (elution solvent:ethyl acetate-hexane (1:50))

出典と根拠

ORDレコード
ord-3b042fa24851427c91e804551dd0d327
出典データセット
uspto-grants-2011_08
特許番号
US07994196B2

関連ノート

読み込み中…