Hydroxyamine hydrochloride → 5-[2-Chloro-4-(trifluoromethyl)phenoxy]2-nitrobenzaldehyde oxime

HRID 1583233ノート

反応式

HRID 1583233 の反応式
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[Cl:9][C:10]1[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:25]=[CH:24][C:11]=1[O:12][C:13]1[CH:14]=[CH:15][C:16]([N+:21]([O-:23])=[O:22])=[C:17]([CH:20]=1)[CH:18]=O>O.C(O)C>[Cl:9][C:10]1[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:25]=[CH:24][C:11]=1[O:12][C:13]1[CH:14]=[CH:15][C:16]([N+:21]([O-:23])=[O:22])=[C:17]([CH:20]=1)[CH:18]=[N:2][OH:3]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 130569775-[2-Chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzaldehyde

生成物 1

HCID 858635775-[2-Chloro-4-(trifluoromethyl)phenoxy]2-nitrobenzaldehyde oxime

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of hydroxylamine hydrochloride (0.33 g., 0.0048 mole) and sodium acetate (0.394 g., 0.0048 mole) in 2-3 ml of water was added a hot solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzaldehyde (1.5 g., 0.00434 mole) in ethanol (10-12 ml). The clear yellow solution was heated for 1.5 hours and then the solvent was stripped on a rotary evaporator to give a yellow waxy solid which solidified giving 1.5 g., mp. 111°-115° C. Recrystallization from ethanol/water gave a solid mp. 114°-118° C.

後処理

  1. temperatureThe clear yellow solution was heated for 1.5 hours
  2. customthe solvent was stripped on a rotary evaporator
  3. customto give a yellow waxy solid which
  4. customsolidified giving 1.5 g
  5. customRecrystallization from ethanol/water

出典と根拠

ORDレコード
ord-7fd3e40ff6e44b9b895c9ade636b1632
出典データセット
uspto-grants-1985_11
特許番号
US04551171

反応ノート

読み込み中…