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Cesium carbonate → Cyclopropanecarboxylic acid {6-[2-(2,6-dichloro-4-cyanophenyl)-2H-pyrazolo[4,3-c]pyridin-4-ylamino]-pyrimidin-4-yl}-amide

HRID 626698
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HRID 626698 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:20])[C:9]=1[N:10]1[CH:19]=[C:13]2[C:14](Cl)=[N:15][CH:16]=[CH:17][C:12]2=[N:11]1)[C:5]#[N:6].[NH2:21][C:22]1[N:27]=[CH:26][N:25]=[C:24]([NH:28][C:29]([CH:31]2[CH2:33][CH2:32]2)=[O:30])[CH:23]=1.CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(#N)C>[OH-:30].[NH4+:6].[Cl:1][C:2]1[CH:3]=[C:4]([C:5]#[N:6])[CH:7]=[C:8]([Cl:20])[C:9]=1[N:10]1[CH:19]=[C:13]2[C:14]([NH:21][C:22]3[N:27]=[CH:26][N:25]=[C:24]([NH:28][C:29]([CH:31]4[CH2:32][CH2:33]4)=[O:30])[CH:23]=3)=[N:15][CH:16]=[CH:17][C:12]2=[N:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 86346445N-(6-Aminopyrimidin-4-yl)cyclopropanecarboxamideHCID 866970463,5-Dichloro-4-(4-chloropyrazolo[4,3-c]pyridin-2-yl)benzonitrile

생성물 2

HCID 14923Ammonium Hydroxide수율 0.1%
HCID 86697047
Cyclopropanecarboxylic acid {6-[2-(2,6-dichloro-4-cyanophenyl)-2H-pyrazolo[4,3-c]pyridin-4-ylamino]-pyrimidin-4-yl}-amide
수율 51.4%

시약·촉매·용매 4

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 962Water용매HCID 6342Acetonitrile용매HCID 312751,4-Dioxane용매

실험 절차

A suspension of 3,5-dichloro-4-(4-chloropyrazolo[4,3-c]pyridin-2-yl)benzonitrile (132 mg, 0.41 mmol), cyclopropanecarboxylic acid (6-amino-pyrimidin-4-yl)-amide (80 mg, 0.45 mmol), Pd2(dba)3 (19 mg, 0.02 mmol), Xantphos (24 mg, 0.04 mmol) and cesium carbonate (266 mg, 0.82 mmol) in dioxane (2 mL) was sealed in a microwave vial after degassing with nitrogen. The mixture was irradiated at 150° C. for 30 minutes in the microwave and then cooled to room temperature. The reaction mixture was partitioned between ethyl acetate and water. The organic layer was separated and washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane), then by HPLC (gradient: 5 to 98% acetonitrile in water with 0.1% ammonium hydroxide), to afford the title compound as an off-white solid (49 mg, 26% yield). 1H NMR (400 MHz, DMSO-d6+d-TFA): δ 9.47 (s, 1H), 8.79 (d, 1H), 8.47 (s, 2H), 8.09 (d, J=0.9 Hz, 1H), 7.99 (d, J=7.6 Hz, 1H), 7.55 (dd, J=7.6, 0.9 Hz, 1H), 2.10-2.02 (m, 1H), 0.93-0.90 (m, 4H). LCMS (Method B): RT=3.17 min, m/z: 465 [M+H+].

후처리

  1. customwas sealed in a microwave vial
  2. customafter degassing with nitrogen
  3. customThe mixture was irradiated at 150° C. for 30 minutes in the microwave
  4. customThe reaction mixture was partitioned between ethyl acetate and water
  5. customThe organic layer was separated
  6. washwashed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane)

출처 및 근거

ORD 기록
ord-f48df1ce121140d2a6dd052cd883b9e5
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09309240B2

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