Hydrochloric Acid → 2-Isopropyl-[1,2,4]triazolo[1,5-a]pyridin-7-amine

HRID 1802197ノート

反応式

HRID 1802197 の反応式
[CH:1]([C:4]1[N:20]=[C:7]2[CH:8]=[C:9]([NH:12]C(=O)OC(C)(C)C)[CH:10]=[CH:11][N:6]2[N:5]=1)([CH3:3])[CH3:2].Cl>O1CCCC1>[CH:1]([C:4]1[N:20]=[C:7]2[CH:8]=[C:9]([NH2:12])[CH:10]=[CH:11][N:6]2[N:5]=1)([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67774335Tert-butyl 2-isopropyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamate

生成物 1

HCID 677763492-Isopropyl-[1,2,4]triazolo[1,5-a]pyridin-7-amine収率 62.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

To a solution of tert-butyl 2-isopropyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamate (400 mg, 1.45 mmol) in tetrahydrofurane (10 ml) is added hydrochloric acid (5 N in diethyl ether, 20 ml, 100 mmol). The resulting suspension is stirred for 18 hours at 25° C. The solvent is evaporated and the residue diluted with ethyl acetate, made basic with sodium hydroxide 2N and washed with water and brine. The organic layer is dried with magnesium sulfate and the solvent is evaporated under reduced pressure. The residue (416 mg) is purified by chromatography on a 20 g silicagel column using heptane/ethyl acetate 50-100% as eluent affording 2-isopropyl-[1,2,4]triazolo[1,5-a]pyridin-7-amine (159 mg, 62.3%) as a white solid. Mp.: 174-6° C. MS: m/z=177.2 (M+H+).

後処理

  1. customThe solvent is evaporated
  2. additionthe residue diluted with ethyl acetate
  3. washwashed with water and brine
  4. dry with materialThe organic layer is dried with magnesium sulfate
  5. customthe solvent is evaporated under reduced pressure
  6. customThe residue (416 mg) is purified by chromatography on a 20 g silicagel column

出典と根拠

ORDレコード
ord-7e5799e48443403bb646a05038fb75ac
出典データセット
uspto-grants-2013_01
特許番号
US08349824B2

反応ノート

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