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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Cesium carbonate → 1-(5-(4-(((1S,9aR)-octahydro-1H-quinolizin-1-yl)methylamino)-5-fluoropyrimidin-2-ylamino)-2-(oxetan-3-yloxy)phenyl)-4-methyl-1H-tetrazol-5(4H)-one

HRID 2175394
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HRID 2175394 반응식
Cl[C:2]1[N:7]=[C:6]([NH:8][CH2:9][C@H:10]2[C@@H:19]3[N:14]([CH2:15][CH2:16][CH2:17][CH2:18]3)[CH2:13][CH2:12][CH2:11]2)[C:5]([F:20])=[CH:4][N:3]=1.[NH2:21][C:22]1[CH:23]=[CH:24][C:25]([O:35][CH:36]2[CH2:39][O:38][CH2:37]2)=[C:26]([N:28]2[C:32](=[O:33])[N:31]([CH3:34])[N:30]=[N:29]2)[CH:27]=1.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.C([O-])([O-])=O.[Cs+].[Cs+]>CC([O-])=O.CC([O-])=O.[Pd+2].O1CCOCC1>[NH3:3].[CH3:32][OH:33].[C@H:10]1([CH2:9][NH:8][C:6]2[C:5]([F:20])=[CH:4][N:3]=[C:2]([NH:21][C:22]3[CH:23]=[CH:24][C:25]([O:35][CH:36]4[CH2:39][O:38][CH2:37]4)=[C:26]([N:28]4[C:32](=[O:33])[N:31]([CH3:34])[N:30]=[N:29]4)[CH:27]=3)[N:7]=2)[C@@H:19]2[N:14]([CH2:15][CH2:16][CH2:17][CH2:18]2)[CH2:13][CH2:12][CH2:11]1
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참가 물질

8

반응물 4

HCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 582872321-(5-amino-2-(oxetan-3-yloxy)phenyl)-4-methyl-1H-tetrazol-5(4H)-oneHCID 867213272-chloro-5-fluoro-N-(((1S,9aR)-octahydro-1H-quinolizin-1-yl)methyl)pyrimidin-4-amine

생성물 2

HCID 21705897Ammonia methanol수율 1%
HCID 86721326
1-(5-(4-(((1S,9aR)-octahydro-1H-quinolizin-1-yl)methylamino)-5-fluoropyrimidin-2-ylamino)-2-(oxetan-3-yloxy)phenyl)-4-methyl-1H-tetrazol-5(4H)-one
수율 76%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 312751,4-Dioxane용매

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온도
120 °C

실험 절차

To a microwave vial, was added 2-chloro-5-fluoro-N-(((1S,9aR)-octahydro-1H-quinolizin-1-yl)methyl)pyrimidin-4-amine (prepared according to Example 1; 400 mg, 1.34 mmol, 1 equiv), 1-(5-amino-2-(oxetan-3-yloxy)phenyl)-4-methyl-1H-tetrazol-5(4H)-one (prepared as described in WO2011/068898, the disclosure of which is incorporated herein by reference; 493 mg, 1.87 mmol, 1.4 equiv), rac-BINAP (181 mg, 0.291 mmol, 0.217 equiv), Cs2CO3 (1.31 g, 4.02 mmol, 3 equiv), Pd(OAc)2 (26 mg, 0.116 mmol, 0.0870 equiv), and dioxane (10 mL). The microwave vial was capped and sonicated under vacuum for 5 min. The reaction mixture was heated in the microwave at 120° C. for 2 h. The cooled reaction mixture was filtered using a pad of celite and rinsed with dioxane, and the filtrate was concentrated. The crude product was purified by flash chromatography and eluted with DCM:2M NH3/MeOH=100:0 to 94:4 using 1% 2M NH3/MeOH increments to provide the desired product Compound 14 1-(5-(4-(((1S,9aR)-octahydro-1H-quinolizin-1-yl)methylamino)-5-fluoropyrimidin-2-ylamino)-2-(oxetan-3-yloxy)phenyl)-4-methyl-1H-tetrazol-5(4H)-one (535 mg, 76%) as a solid.

후처리

  1. customprepared
  2. customThe microwave vial was capped
  3. customsonicated under vacuum for 5 min
  4. customThe cooled reaction mixture
  5. filtrationwas filtered
  6. washrinsed with dioxane
  7. concentrationthe filtrate was concentrated
  8. customThe crude product was purified by flash chromatography
  9. washeluted with DCM

출처 및 근거

ORD 기록
ord-386b895c4bc2439fa028d271ad8c07dd
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09062068B2

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