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Hydrochloric Acid → 2-Chloro-5-(5-oxo-1,5-dihydro-[1,2,4]triazol-4-yl)-benzoic acid

HRID 1767579
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반응식

HRID 1767579 반응식
[CH:1]([NH:3][NH:4][C:5]([NH:7][C:8]1[CH:13]=[C:12]([C:14]([O:16]C)=[O:15])[CH:11]=[CH:10][C:9]=1Cl)=[O:6])=O.[ClH:19]>[OH-].[K+].CO>[Cl:19][C:11]1[CH:10]=[CH:9][C:8]([N:7]2[C:5](=[O:6])[NH:4][N:3]=[CH:1]2)=[CH:13][C:12]=1[C:14]([OH:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 210939021-Formyl-4-(2-chloro-5-carbomethoxyphenyl)semicarbazide

생성물 1

HCID 210939062-Chloro-5-(5-oxo-1,5-dihydro-[1,2,4]triazol-4-yl)-benzoic acid수율 100%

시약·촉매·용매 2

HCID 887Methanol용매HCID 14797Potassium Hydroxide용매

실험 절차

A solution of 1-formyl-4-(2-chloro-5-carbomethoxyphenyl)semicarbazide (0.03 g, 0.11 mmol) in 1.0 M KOH in methanol (MeOH) (0.44 mL) was heated at 80° C. for 72 hours and cooled to room temperature. 1.0 N HCl (0.8 mL) was added and the mixture evaporated to dryness in vacuo. The residue was taken up in MeOH (1.5 mL) and filtered. The filtrate was concentrated in vacuo to yield 0.028 g (100%) of the title intermediate as an amorphous solid. Mass Spectrum (M−H): 3:1 ratio of 238 and 240.

후처리

  1. customthe mixture evaporated to dryness in vacuo
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-f86256d62a1c4dbfb05d7cc9aef022f1
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07235549B2

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