Hydrochloric Acid → 4-chloro-N,2-dihydroxybenzamide

HRID 259669

반응식

HRID 259669 반응식
Cl.[NH2:2][OH:3].C[O-].[Na+].[Cl:7][C:8]1[CH:9]=[C:10]([OH:18])[C:11](=[CH:16][CH:17]=1)[C:12](OC)=[O:13].Cl>CO>[Cl:7][C:8]1[CH:9]=[C:10]([OH:18])[C:11](=[CH:16][CH:17]=1)[C:12]([NH:2][OH:3])=[O:13]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 327085Methyl 4-chloro-2-hydroxybenzoateHCID 443297Hydroxyamine hydrochlorideHCID 10942334Sodium Methoxide

생성물 1

HCID 27818484-chloro-N,2-dihydroxybenzamide

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

Hydroxylamine hydrochloride (20.65 g, 0.297 mol) is added to a mixture of sodium methoxide (53 g, 0.99 mol) in methanol while maintaining the temperature below 10° C. A mixture of methyl 4-chlorosalicylate (46.2 g, 0.248 mol) in methanol is then added to the reaction mixture and the resultant mixture is stirred at room temperature for 10 days, acidified with concentrated hydrochloric acid (pH3) and filtered to give the title product as an off-white solid which is identified by NMR spectral analyses.

후처리

  1. temperaturewhile maintaining the temperature below 10° C
  2. additionis then added to the reaction mixture
  3. filtrationfiltered

출처 및 근거

ORD 기록
ord-89b5131461cb4552905ee45876d6a515
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05523278

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