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1-Cyanocyclohexylamine hydrochloride → HCID 24772730, 화합물

HRID 1696173
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HRID 1696173 반응식
[C:1]([C:4]1[CH:5]=[N:6][N:7]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=3)=[C:11]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[Cl:26])[CH:10]=[N:9][C:8]=12)(O)=[O:2].Cl.[C:28]([C:30]1([NH2:36])[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1)#[N:29].O.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.CN(C)C=O.C(N(CC)CC)C.O>[Cl:26][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[C:11]1[CH:10]=[N:9][C:8]2[N:7]([N:6]=[CH:5][C:4]=2[C:1](=[O:2])[NH:36][C:30]2([C:28]#[N:29])[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)[C:12]=1[C:13]1[CH:14]=[CH:15][C:16]([Cl:19])=[CH:17][CH:18]=1
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참가 물질

10

반응물 5

HCID 1982621-Cyanocyclohexylamine hydrochlorideHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 67272265HCID 67272265, 화합물

생성물 1

HCID 24772730HCID 24772730, 화합물
수율 21.1%

시약·촉매·용매 4

HCID 962Water용매HCID 6212Chloroform용매3회HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

실험 절차

To a solution of 3-carboxy-6-(2-chlorophenyl)-7-(4-chlorophenyl)pyrazolo-[1,5-a]pyrimidine (compound obtained in Reference Example 1-(4); 58 mg) and 1-cyanocyclohexylamine hydrochloride (25 mg) in chloroform (1.0 mL containing amylene) were added a 0.5 M solution of 1-hydroxybenzotriazole monohydrate in chloroform (0.45 mL containing amylene), a 0.5 M solution of 1-(3-dimethylamino-propyl)-3-ethylcarbodiimide hydrochloride in N,N-dimethylformamide (0.45 mL) and triethylamine (63 μL), and the mixture was stirred at room temperature overnight. To the reaction mixture were added an aqueous saturated sodium hydrogencarbonate solution (2 mL), water (2 mL) and chloroform (4 mL), and the mixture was vigorously stirred for 15 minutes. The organic layer was separated, and the aqueous layer was extracted with chloroform (3 mL). The combined organic layer was washed successively with an aqueous saturated sodium hydrogencarbonate solution (3 mL) and brine (3 mL) and concentrated in vacuo. The resultant crude product was purified by liquid chromatograph-mass spectrometer (LCMS, column; XTerra MS C18, solvent; 10 mM ammonium carbonate/methanol 40/60 to 10/90) and lyophilized to give 6-(2-chlorophenyl)-7-(4-chlorophenyl)-3-[N-(1-cyanocyclohexyl)carbamoyl]pyrazolo[1,5-a]pyrimidine (15.6 mg; yield: 21%) as a powder.

후처리

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted with chloroform (3 mL)
  3. washThe combined organic layer was washed successively with an aqueous saturated sodium hydrogencarbonate solution (3 mL) and brine (3 mL)
  4. concentrationconcentrated in vacuo
  5. customThe resultant crude product was purified by liquid chromatograph-mass spectrometer (LCMS, column; XTerra MS C18, solvent; 10 mM ammonium carbonate/methanol 40/60 to 10/90)

출처 및 근거

ORD 기록
ord-bd72c6172b0944b3992a51caa522dd21
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163759B2

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