1-Chloro-2,4-Dinitrobenzene → 2-(2,4-Dinitrophenoxy)ethanol

HRID 1531476

反応式

HRID 1531476 の反応式
[C:1]([O-:5])(=O)[CH2:2][OH:3].C=C.[K+].[N+:9]([C:12]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=1Cl)([O-:11])=[O:10].O>C(O)CO>[N+:9]([C:12]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:13]=1[O:3][CH2:2][CH2:1][OH:5])([O-:11])=[O:10]

参加物

5

反応物 3

HCID 61-Chloro-2,4-DinitrobenzeneHCID 962WaterHCID 86756524Mono-potassium ethylene glycolate2 回

生成物 1

HCID 760702-(2,4-Dinitrophenoxy)ethanol収率 92%

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒2 回

反応条件

温度
65 °C

実験手順

200 ml of ethylene glycol and 40 ml of the mono-potassium ethylene glycolate solution prepared under Example 3 were introduced initially under nitrogen and were heated to 65° C. in a 2 l reaction vessel fitted with a stirrer. Over the course of 5 h, 162 g of molten 2,4-dinitro-chloro-benzene and the remainder of the mono-potassium ethylene glycolate solution in ethylene glycol were simultaneously metered in. The mixture was then stirred for one hour at 65° C., and then 600 ml of water were added. The precipitate which formed was filtered off and washed with 1000 ml of water and dried, giving 169.7 g of 2-(2′,4′-dinitrophenoxy)-ethanol in a purity of 92%. Hence, a yield of 92% is achieved based on 2,4-dinitrochlorobenzene.

後処理

  1. additionwere introduced initially under nitrogen
  2. customfitted with a stirrer
  3. customThe precipitate which formed
  4. filtrationwas filtered off
  5. washwashed with 1000 ml of water
  6. customdried

出典と根拠

ORDレコード
ord-f398d6fb983c4ef7a14e7d638084023a
出典データセット
uspto-grants-2001_03
特許番号
US06198007B1

関連ノート

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