Hydrochloric Acid → 3-(3-Phenyl-1H-1,2,4-triazol-1-yl)propionoic acid

HRID 1621103노트

반응식

HRID 1621103 반응식
[C:1]1([C:7]2[N:11]=[CH:10][NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:13][CH2:14][C:15]([OH:17])=[O:16].[OH-].[Na+].Cl>O>[C:1]1([C:7]2[N:11]=[CH:10][N:9]([CH2:13][CH2:14][C:15]([OH:17])=[O:16])[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 78993-Chloropropionic acid2회HCID 14798Sodium Hydroxide2회HCID 178420160HCID 178420160, 화합물

생성물 1

HCID 124615483-(3-Phenyl-1H-1,2,4-triazol-1-yl)propionoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
115 °C

실험 절차

A mixture of 3-phenyl-1H-1,2,4-triazole (1.46 g, 9.05 mmol), 3-chloropropionic acid (1.08 g, 9.96 mmol) and sodium hydroxide (2M, 9.05 mL, 18.1 mmol) in water (3 mL) was heated to 115° C. and stirred for 66 h. Another 0.5 equivalents of each 3-chloropropanoic acid and sodium hydroxide were added (pH increase to 11) and stirring was continued for another 24 h. Hydrochloric acid (2M, 10 mL) was added, the suspension was filtered and extracted with dichloromethane. The product was obtained after purification by supercritical fluid chromatography as light brown solid (236 mg, 1.09 mmol, 12.0%). MS: M=218.1 (M+H)+

후처리

  1. temperaturepH increase to 11) and
  2. stirringstirring
  3. waitwas continued for another 24 h
  4. filtrationthe suspension was filtered
  5. extractionextracted with dichloromethane
  6. customThe product was obtained

출처 및 근거

ORD 기록
ord-fece11ea03634350a893b80cc94d85f4
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772510B2

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