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

HRID 1621103ノート

反応式

HRID 1621103 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 78993-Chloropropionic acid2 回HCID 14798Sodium Hydroxide2 回HCID 178420160HCID 178420160、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
115 °C

実験手順

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)+

後処理

  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

出典と根拠

ORDレコード
ord-fece11ea03634350a893b80cc94d85f4
出典データセット
uspto-grants-2014_07
特許番号
US08772510B2

反応ノート

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