Hydrochloric Acid → Benzoic acid, 2-[(2-bromophenyl)thio]-5-nitro-

HRID 33803

반응식

HRID 33803 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].[OH-].[K+].F[C:12]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:13]=1[C:14]([OH:16])=[O:15].Cl>O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][C:12]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:13]=1[C:14]([OH:16])=[O:15]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 805982-BromobenzenethiolHCID 2809972-Fluoro-5-nitrobenzoic acid

생성물 1

HCID 43090919Benzoic acid, 2-[(2-bromophenyl)thio]-5-nitro-수율 99%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-Bromobenzenethiol (7.2 ml, 85.9 mmol) was added to a solution of KOH (9.6 g, 172 mmol) in water (50 ml) degassed for 15 minutes. 2-Fluoro-5-nitrobenzoic acid (15.9 g, 85.9 mmol) was added to the reaction mixture, which was refluxed under a nitrogen atmosphere overnight. The reaction was cooled to room temperature and was acidified (pH 1) with conc. HCl. The precipitate formed was filtered and dried overnight in a vacuum oven (50° C.) to give the crude title compound as a pale yellow solid (30 g, 99%). The product was used without further purification. m/z (LC-MS, ESP), RT=4.51min, (M−−1)=352-354, (1:1, bromine isotope ratio present).

후처리

  1. customdegassed for 15 minutes
  2. temperaturewas refluxed under a nitrogen atmosphere overnight
  3. customThe precipitate formed
  4. filtrationwas filtered
  5. customdried overnight in a vacuum oven (50° C.)

출처 및 근거

ORD 기록
ord-d76cec926c5e4cbd8ab02ae004f84f9b
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429660B2

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