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Sulfuric Acid → HCID 86685630, 화합물

HRID 332840
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HRID 332840 반응식
Cl[C:2]1[N:7]=[C:6]([NH:8][C@@H:9]2[CH2:14][CH2:13][CH2:12][CH2:11][C@@H:10]2[NH:15]C(=O)[O-])[CH:5]=[N:4][C:3]=1[C:19]#[N:20].[N:21]1[CH:26]=[CH:25][CH:24]=[N:23][C:22]=1[C:27]1[CH:28]=[C:29]([NH2:33])[CH:30]=[N:31][CH:32]=1.C(=O)([O-])[O-:35].[Cs+].[Cs+].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.OS(O)(=O)=O>O1CCOCC1.C(O)(C(F)(F)F)=O.O.CC([O-])=O.CC([O-])=O.[Pd+2]>[NH2:15][C@H:10]1[CH2:11][CH2:12][CH2:13][CH2:14][C@H:9]1[NH:8][C:6]1[N:7]=[C:2]([NH:33][C:29]2[CH:30]=[N:31][CH:32]=[C:27]([C:22]3[N:23]=[CH:24][CH:25]=[CH:26][N:21]=3)[CH:28]=2)[C:3]([C:19]([NH2:20])=[O:35])=[N:4][CH:5]=1
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참가 물질

10

반응물 5

HCID 1118Sulfuric AcidHCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 69284611HCID 69284611, 화합물HCID 86685625((1S,2R)-2-((6-chloro-5-cyanopyrazin-2-yl)amino)cyclohexyl)carbamate

생성물 1

HCID 86685630HCID 86685630, 화합물수율 30.8%

시약·촉매·용매 4

HCID 167845palladium(II) acetate촉매HCID 962Water용매HCID 6422Trifluoroacetic acid용매HCID 312751,4-Dioxane용매

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온도
110 °C

실험 절차

The mixture of tert-tutyl ((1S,2R)-2-((6-chloro-5-cyanopyrazin-2-yl)amino)cyclohexyl)carbamate (100 mg, 0.28 mmol), 5-(pyrimidin-2-yl)pyridin-3-amine (100 mg, 0.58 mmol), powder cesium carbonate (380 mg, 1.16 mmol), BINAP (37 mg, 0.06 mmol), Pd(OAc)2 (14 mg, 0.06 mmol) in 15 mL dioxane was degassed with argon stream. It was stirred in argon atmosphere at 110° C. for overnight. The mixture was cooled, diluted with 100 mL EtOAc, vigorously stirred, and filtered through celite. The filtrate was concentrated and subjected to silica flash column with 20-100% EtOAc in DCM to isolate the coupling product. It was then stirred in 5 mL TFA and 1 mL conc. H2SO4 at 80° C. for 30 m. It was cooled in ice bath, diluted with water, filtered, and subjected to reverse phase preparative HPLC to isolate the title compound (35 mg). MS found for C20H23N90 as (M+H)+ 406.5. UV: λ=259, 306 nm. 1H NMR: (CD3OD) δ 9.63 (1H, s), 9.24 (1H, s), 9.02 91H, s), 8.98 (2H, d, J=4.4 Hz), 7.70 (1H, s), 7.53 (1H, t, J=4.8 Hz), 4.74 (1H, m), 3.69 (1H, m), 1.92-1.56 (8H, m) ppm.

후처리

  1. customwas degassed with argon stream
  2. temperatureThe mixture was cooled
  3. additiondiluted with 100 mL EtOAc
  4. stirringvigorously stirred
  5. filtrationfiltered through celite
  6. concentrationThe filtrate was concentrated
  7. customto isolate the coupling product
  8. customat 80° C.
  9. temperatureIt was cooled in ice bath
  10. filtrationfiltered

출처 및 근거

ORD 기록
ord-40c124915e894518be0b0e99932a6417
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08877760B2

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