Hydrochloric Acid → 3-(1H-pyrazol-4-yl)-pyridin-2-ylamine

HRID 77865노트

반응식

HRID 77865 반응식
C([N:20]1[CH:24]=[C:23]([C:25]2[C:26]([NH2:31])=[N:27][CH:28]=[CH:29][CH:30]=2)[CH:22]=[N:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.Cl.CO>O1CCCC1>[NH:20]1[CH:24]=[C:23]([C:25]2[C:26]([NH2:31])=[N:27][CH:28]=[CH:29][CH:30]=2)[CH:22]=[N:21]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 592552153-(1-Trityl-1H-pyrazol-4-yl)-pyridin-2-ylamine

생성물 1

HCID 592552903-(1H-pyrazol-4-yl)-pyridin-2-ylamine수율 68.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

3-(1-Trityl-1H-pyrazol-4-yl)-pyridin-2-ylamine (2.3 g, 5.71 mmol) described in Manufacturing Example 32-1-3, 2 N hydrochloric acid (15 mL), methanol (15 mL) and tetrahydrofuran (10 mL) were stirred for 30 minutes at 70° C. The reaction solution was allowed to room temperature, and partitioned into water and ethyl acetate. Saturated sodium bicarbonate solution was added to the separated aqueous layer, which was then extracted with ethyl acetate 6 times. The ethyl acetate layers were combined and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate, then ethyl acetate: methanol=10:1) to obtain the title compound (625 mg, 68.3%).

후처리

  1. customwas allowed to room temperature
  2. custompartitioned into water and ethyl acetate
  3. additionSaturated sodium bicarbonate solution was added to the separated aqueous layer, which
  4. extractionwas then extracted with ethyl acetate 6 times
  5. customthe solvent was evaporated under a reduced pressure
  6. customThe residue was purified by silica gel chromatography (ethyl acetate

출처 및 근거

ORD 기록
ord-81d052e35a594accba6a56cbed8a6d02
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841327B2

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