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

HRID 1461258
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HRID 1461258 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f721b0078c8f4cfd8a99c63807fa07b5
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05075304

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