Hydrochloric Acid → N2,N2-dimethyl-[1,2,4]triazolo[1,5-a]pyridine-2,7-diamine

HRID 1802204ノート

反応式

HRID 1802204 の反応式
[CH3:1][N:2]([CH3:20])[C:3]1[N:19]=[C:6]2[CH:7]=[C:8]([NH:11]C(=O)OC(C)(C)C)[CH:9]=[CH:10][N:5]2[N:4]=1.Cl>ClCCl>[CH3:1][N:2]([CH3:20])[C:3]1[N:19]=[C:6]2[CH:7]=[C:8]([NH2:11])[CH:9]=[CH:10][N:5]2[N:4]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67775938Tert-butyl 2-(dimethylamino)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamate

生成物 1

HCID 67774846N2,N2-dimethyl-[1,2,4]triazolo[1,5-a]pyridine-2,7-diamine収率 63.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of tert-butyl 2-(dimethylamino)-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamate (1.8 g, 6.49 mmol) in dichloromethane (15 ml) and hydrochloric acid (5N in diethyl ether, 50 ml, 250 mmol) is stirred for 18 hours at room temperature. The solvent is evaporated and the residue dissolved in water (100 ml), made basic with 32% aqueous sodium hydroxide and extracted twice with ethyl acetate. The combined organic layers are washed with water, dried with magnesium sulfate and the solvent is evaporated under reduced pressure affording N2,N2-dimethyl-[1,2,4]triazolo[1,5-a]pyridine-2,7-diamine (727 mg, 63.2%) as a yellow solid. Mp.: 236-8° C. MS: m/z=178.1 (M+H+).

後処理

  1. customThe solvent is evaporated
  2. dissolutionthe residue dissolved in water (100 ml)
  3. extractionextracted twice with ethyl acetate
  4. washThe combined organic layers are washed with water
  5. dry with materialdried with magnesium sulfate
  6. customthe solvent is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-e815509e6e9d458185dc035b73cb0a66
出典データセット
uspto-grants-2013_01
特許番号
US08349824B2

反応ノート

読み込み中…