Nitric Acid → 3-Nitro-2,5,6-trichlorobenzoic acid

HRID 487194

반응식

HRID 487194 반응식
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([Cl:12])[C:3]=1[C:4]([OH:6])=[O:5].[N+:13]([O-])([OH:15])=[O:14]>S(=O)(=O)(O)O>[N+:13]([C:8]1[C:7]([Cl:12])=[C:3]([C:2]([Cl:1])=[C:10]([Cl:11])[CH:9]=1)[C:4]([OH:6])=[O:5])([O-:15])=[O:14]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 57592,3,6-Trichlorobenzoic acid

생성물 1

HCID 190942393-Nitro-2,5,6-trichlorobenzoic acid수율 94%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매3회

반응 조건

온도
43 °C

실험 절차

2,3,6-Trichlorobenzoic acid (20.84 g, 92.4 mmol, prepared by the method of M. T. Goebel, U.S. Pat. No. 3,391,185, E.I. DuPont, Jul. 2, 1968) was stirred at 40°-45° C. in 89.1 mL of concentrated sulfuric acid. A solution containing 23.2 g of concentrated sulfuric acid and 23.2 g of fuming nitric acid was added at a rate so to maintain the temperature between 40°-45° C. An additional 20 mL of concentrated sulfuric acid was added. The reaction mixture was stirred at 43° C. for 1.5 hours and then poured over ice water. The resulting crystals were filtered and recrystallized from toluene-hexane to give 23.40 g (94%) of product; mp 149°-151° C.

후처리

  1. additionwas added at a rate so
  2. temperatureto maintain the temperature between 40°-45° C
  3. filtrationThe resulting crystals were filtered
  4. customrecrystallized from toluene-hexane

출처 및 근거

ORD 기록
ord-2af3472b9a024c70bc69434d4d87d6a0
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05294631

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