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Sodium Carbonate → HCID 117667280、化合物

HRID 712724
ノート
印刷プレビュー

反応式

HRID 712724 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 1

HCID 117667280HCID 117667280、化合物

試薬・触媒・溶媒 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒2 回HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-35f32584132b4e9099f800c59c453418
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181272B2

反応ノート

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