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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Carbonate → HCID 117667280, 화합물

HRID 712724
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HRID 712724 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[NH:8][CH2:7][CH2:6][CH2:5]2.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C([O-])(=O)C.[K+].Br[C:36]1[CH:37]=[N:38][CH:39]=[C:40]([F:46])[C:41]=1[C:42]([OH:45])([CH3:44])[CH3:43].C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[F:46][C:40]1[CH:39]=[N:38][CH:37]=[C:36]([C:2]2[CH:11]=[N:10][C:9]3[NH:8][CH2:7][CH2:6][CH2:5][C:4]=3[CH:3]=2)[C:41]=1[C:42]([OH:45])([CH3:43])[CH3:44]
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참가 물질

8

반응물 5

HCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 179301266-Bromo-1,2,3,4-tetrahydro-1,8-naphthyridineHCID 671550712-(3-Bromo-5-fluoropyridin-4-yl)propan-2-ol

생성물 1

HCID 117667280HCID 117667280, 화합물

시약·촉매·용매 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매2회HCID 312751,4-Dioxane용매

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온도
120 °C

실험 절차

To a vial is added 6-bromo-1,2,3,4-tetrahydro-[1,8]naphthyridine, Intermediate A (144 mg, 0.68 mmol), bis(pinacolato)diboron (223 mg, 0.88 mmol), potassium acetate (200 mg, 2 mmol) and [1,1′-bis(diphenylphosphino)ferrocene)dichloropalladium(II) (50 mg, 0.07 mmol) in 5 ml of 1,4-dioxane. The reaction mixture is stirred at 120° C. under Ar for 2 hours. The reaction mixture is cooled down to room temperature, followed by the addition of 2-(3-bromo-5-fluoro-pyridin-4-yl)-propan-2-ol (190 mg, 0.81 mmol), 2M Na2CO3 (0.67 ml, 1.35 mmol) and [1,1′-bis(diphenylphosphino)ferrocene)dichloropalladium(II) (25 mg, 0.034 mmol). The reaction mixture is stirred under Ar at 120° C. for 3 hours. The reaction mixture is concentrated. The residue is diluted with EtOAc, washed with water, brine, dried over anhydrous Na2SO4, filtered and concentrated to give the crude product. Purification by the flash column chromatography affords 72 mg of 2-[3-fluoro-5-(5,6,7,8-tetrahydro-[1,8]naphthyridin-3-yl)-pyridin-4-yl]-propan-2-ol.

후처리

  1. temperatureThe reaction mixture is cooled down to room temperature
  2. stirringThe reaction mixture is stirred under Ar at 120° C. for 3 hours
  3. concentrationThe reaction mixture is concentrated
  4. additionThe residue is diluted with EtOAc
  5. washwashed with water, brine
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give the crude product
  10. customPurification by the flash column chromatography

출처 및 근거

ORD 기록
ord-35f32584132b4e9099f800c59c453418
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181272B2

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