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

HRID 1802139

반응식

HRID 1802139 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-6ad8e7224305471dab0873492dc88cd7
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349824B2

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