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Nitric Acid → 5-Chloro-2-ethoxalylamino-3-nitrobenzotrifluoride

HRID 1461258
ノート
印刷プレビュー

反応式

HRID 1461258 の反応式
[C:1]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][C:10]=1[C:16]([F:19])([F:18])[F:17])([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:2].[N+:20]([O-])([OH:22])=[O:21]>S(=O)(=O)(O)O>[C:1]([NH:8][C:9]1[C:14]([N+:20]([O-:22])=[O:21])=[CH:13][C:12]([Cl:15])=[CH:11][C:10]=1[C:16]([F:17])([F:18])[F:19])([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 944Nitric AcidHCID 4550962Ethyl 2-[4-chloro-2-(trifluoromethyl)anilino]-2-oxoacetate

生成物 1

HCID 199803055-Chloro-2-ethoxalylamino-3-nitrobenzotrifluoride

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

A solution of N-ethoxalyl-4-chloro-2-trifluoromethylaniline in concentrated sulphuric acid (125 ml) was added to a stirred mixture of 100% nitric acid (120 ml) and concentrated sulphuric acid (240 ml). The temperature was kept between 8°-10° C. during the addition. After the addition was completed, the solution was stirred for additionally 20 min. without external cooling, whereafter it was poured onto icewater. This afforded precipitation of the title compound as an oil, which crystallized as light yellow crystals upon standing. The crystals were filtered off and washed extensively with water. M.p. 100°-101° C.

後処理

  1. additionThe temperature was kept between 8°-10° C. during the addition
  2. additionAfter the addition
  3. additionwas poured onto icewater
  4. customThis afforded precipitation of the title compound as an oil, which
  5. customcrystallized as light yellow crystals
  6. filtrationThe crystals were filtered off
  7. washwashed extensively with water

出典と根拠

ORDレコード
ord-f721b0078c8f4cfd8a99c63807fa07b5
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05075304

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート