Water → 2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine

HRID 1802139

反応式

HRID 1802139 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][N:11]2[N:14]=[C:15]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[N:16]=[C:10]2[CH:9]=1)(C)(C)C.O.C(OCC)(=O)C>Cl>[C:17]1([C:15]2[N:16]=[C:10]3[CH:9]=[C:8]([NH2:7])[CH:13]=[CH:12][N:11]3[N:14]=2)[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参加物

5

反応物 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 67773976(2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-carbamic acid tert-butyl ester

生成物 1

HCID 677741452-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine収率 95.9%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A suspension of (2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-carbamic acid tert-butyl ester (8.5 g, 27.4 mmol) in hydrochloric acid (6 N in diethyl ether, 175 ml) is stirred overnight at room temperature. The suspension is diluted under cooling with water (ca 2 l) and ethyl acetate, the aqueous layer is washed once with ethyl acetate, made alkaline with 32% aqueous sodium hydroxide and extracted twice with ethyl acetate. The combined organic layers are dried with magnesium sulfate and the solvent is removed in vacuo affording 2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine (5.52 g, 95.9%) as a light pink solid. mp.: 212-213° C. MS: m/z=211.2 (M+H+).

後処理

  1. additionThe suspension is diluted
  2. washthe aqueous layer is washed once with ethyl acetate
  3. extractionextracted twice with ethyl acetate
  4. dry with materialThe combined organic layers are dried with magnesium sulfate
  5. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-6ad8e7224305471dab0873492dc88cd7
出典データセット
uspto-grants-2013_01
特許番号
US08349824B2

関連ノート

読み込み中…