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Sodium Carbonate → HCID 117667664, 화합물

HRID 712692
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HRID 712692 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[N:8]([C:12]([NH2:14])=[O:13])[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:39]1[CH:40]=[C:41]([C:45]2([OH:49])[CH2:48][O:47][CH2:46]2)[CH:42]=[N:43][CH:44]=1.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]>[OH:49][C:45]1([C:41]2[CH:40]=[C:39]([C:2]3[CH:3]=[C:4]4[C:9](=[N:10][CH:11]=3)[N:8]([C:12]([NH2:14])=[O:13])[CH2:7][CH2:6][CH2:5]4)[CH:44]=[N:43][CH:42]=2)[CH2:48][O:47][CH2:46]1
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참가 물질

8

반응물 5

HCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 754066851432621-15-2HCID 117667602HCID 117667602, 화합물

생성물 1

HCID 117667664HCID 117667664, 화합물수율 6.3%

시약·촉매·용매 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매2회
HCID 312751,4-Dioxane용매2회

반응 조건

온도
80 °C

실험 절차

A vial containing 6-bromo-3,4-dihydro-2H-[1,8]naphthyridine-1-carboxylic acid amide (350 mg, 1.4 mmol), bis(pinacolato)diboron (573 mg, 2.3 mmol), 1,1′-bis(diphenylphosphino)ferrocenedichloropalladium (II) (50 mg, 0.068 mmol) and potassium acetate (604 mg, 6.2 mmol) in 1,4-dioxane (10 mL) is flushed with Ar, sealed tightly and heated to 80° C. for 2 h. The reaction mixture is cooled to room temperature and a solution of 3-(5-bromo-pyridin-3-yl)-oxetan-3-ol (314 mg, 1.37 mmol) in 1,4-dioxane (4 mL), aqueous sodium carbonate solution (2M, 1.4 mL, 2.7 mmol) and additional 1,1′-bis(diphenylphosphino)ferrocenedichloropalladium (II) (50 mg, 0.068 mmol) are added. The mixture is flushed with Ar, sealed tightly and heated to 100° C. for 90 min. After cooling to room temperature the mixture is partitioned between water and EtOAc. The layers are separated and the aqueous is further extracted with EtOAc. The combined organic layers are washed with brine, dried (Na2SO4) and concentrated. To the residue is added MeOH to form a precipitate which is collected by filtration to afford the title compound (28 mg).

후처리

  1. customis flushed with Ar
  2. customsealed tightly
  3. temperatureThe reaction mixture is cooled to room temperature
  4. customThe mixture is flushed with Ar
  5. customsealed tightly
  6. temperatureheated to 100° C. for 90 min
  7. temperatureAfter cooling to room temperature the mixture
  8. customis partitioned between water and EtOAc
  9. customThe layers are separated
  10. extractionthe aqueous is further extracted with EtOAc
  11. washThe combined organic layers are washed with brine
  12. dry with materialdried (Na2SO4)
  13. concentrationconcentrated
  14. additionTo the residue is added MeOH
  15. customto form a precipitate which
  16. filtrationis collected by filtration

출처 및 근거

ORD 기록
ord-2fc45fcae2334ecd9384057d737bd04c
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181272B2

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