Hydrochloric Acid → HCID 68282941, 화합물

HRID 624034노트

반응식

HRID 624034 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=O)[CH2:10][N:11]2[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[N:12]2)=[N:6][CH:7]=1.Cl>C1COCC1.CCOC(C)=O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][CH2:9][CH2:10][N:11]2[CH:15]=[C:14]([N+:16]([O-:18])=[O:17])[CH:13]=[N:12]2)=[N:6][CH:7]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 68283437HCID 68283437, 화합물

생성물 1

HCID 68282941HCID 68282941, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매3회HCID 8857Ethyl Acetate용매

실험 절차

To N-(5-fluoropyridin-2-yl)-2-(4-nitro-1H-pyrazol-1-yl)acetamide (493 mg) in THF (2.0 mL), BH3 THF-complex solution (1 M in THF, 7.3 mL, 7.3 mmol) was added dropwise. After stirring at rt for 3 h, the reaction mixture was quenched with 1 N aq. HCl-solution (3 mL, 3 mmol). The mixture was stirred for 15 min at rt, and heated to 60° C. for 1.5 h. The reaction mixture was diluted with EtOAc, washed with sat. aq. Na2CO3-solution. The aq. layer was reextracted with EtOAc and the comb. org. layers were evaporated, dissolved in DCM and washed with brine. The org. layer was dried (MgSO4), filtered and the solvent was removed by reduced pressure to yield 5-fluoro-N-(2-(4-nitro-1H-pyrazol-1-yl)ethyl)pyridin-2-amine as a yellow solid. LC-MS conditions A: tR=0.53 min, [M+H]+=252.36.

후처리

  1. stirringThe mixture was stirred for 15 min at rt
  2. temperatureheated to 60° C. for 1.5 h
  3. washwashed with sat. aq. Na2CO3-solution
  4. customlayers were evaporated
  5. dissolutiondissolved in DCM
  6. washwashed with brine
  7. dry with materiallayer was dried (MgSO4)
  8. filtrationfiltered
  9. customthe solvent was removed by reduced pressure

출처 및 근거

ORD 기록
ord-09856ca05786485782ea34783f9f5fd1
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303023B2

반응 노트

불러오는 중…