Cyclohexylamine → ethyl 4-cyclohexylamino-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate

HRID 1966802노트

반응식

HRID 1966802 반응식
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[C:9]1[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][N:12]=[C:11]2[N:20]([CH2:23][CH3:24])[N:21]=[CH:22][C:10]=12>C(#N)C>[CH:1]1([NH:7][C:9]2[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][N:12]=[C:11]3[N:20]([CH2:23][CH3:24])[N:21]=[CH:22][C:10]=23)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 7965CyclohexylamineHCID 10491120ethyl 4-chloro-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate

생성물 1

HCID 10448469ethyl 4-cyclohexylamino-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
110 °C

실험 절차

Cyclohexyl amine (9.07 ml, 0.7905 mole) was added to a mixture of ethyl 4-chloro-1-ethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate (10 gm, 0.0395 mole) (example 3) in acetonitrile. After stirring for about 2 h at 110° C., acetonitrile was removed under reduced pressure. Water was added and the reaction mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulphate and concentrated in vacuo to give brownish solid.

후처리

  1. customacetonitrile was removed under reduced pressure
  2. additionWater was added
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated in vacuo
  7. customto give brownish solid

출처 및 근거

ORD 기록
ord-46412d01f50f48dda4dae1df5fd9a5de
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08420666B2

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