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Nitric Acid → HCID 10379608, 화합물

HRID 640797
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HRID 640797 반응식
[C:1]([NH:4][C:5]1[C:6]([Cl:15])=[CH:7][C:8]([Cl:14])=[C:9]([CH:13]=1)[C:10]([OH:12])=[O:11])(=[O:3])[CH3:2].[N+:16]([O-])([OH:18])=[O:17]>S(=O)(=O)(O)O>[C:1]([NH:4][C:5]1[C:13]([N+:16]([O-:18])=[O:17])=[C:9]([C:8]([Cl:14])=[CH:7][C:6]=1[Cl:15])[C:10]([OH:12])=[O:11])(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric Acid2회HCID 2833165-(Acetylamino)-2,4-dichlorobenzoic acid

생성물 1

HCID 10379608HCID 10379608, 화합물수율 86%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

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온도
0 °C

실험 절차

5-Acetamido-2,4-dichlorobenzoic acid (9.6 g, 0.039 mol) was added in small portions over 30 min to a stirred ice-cooled solution of fuming nitric acid (1.8 mL, 0.043 mol) and conc sulfuric acid (120 mL). After the addition was complete, more fuming nitric acid (17 mL) and conc sulfuric acid (80 mL) were added at 30 min and 60 min intervals. The reaction mixture was then left to stir for an additional 2.5 h at 0° C., allowed to warm to 12-16° C. and left to stir at this temperature until all starting material was consumed (about 3 h). The solution was poured onto ice and extracted with ethyl acetate (3×). The organic extracts were combined, washed with brine, dried, and concentrated to give 3-acetamido-4,6-dichloro-2-nitrobenzoic acid as an orange solid (9.8 g, 86%).

후처리

  1. additionAfter the addition
  2. waitThe reaction mixture was then left
  3. temperatureto warm to 12-16° C.
  4. waitleft
  5. stirringto stir at this temperature until all starting material
  6. customwas consumed (about 3 h)
  7. additionThe solution was poured onto ice
  8. extractionextracted with ethyl acetate (3×)
  9. washwashed with brine
  10. customdried
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c98c552c8ef945679f88f5ea803d7007
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07692011B2

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