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Potassium Carbonate → HCID 89862967, 화합물

HRID 1053681
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HRID 1053681 반응식
Br[C:2]1[CH:3]=[C:4]([C@H:8]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])[CH3:9])[CH:5]=[CH:6][CH:7]=1.CC1(C)C(C)(C)OB([C:26]2[CH:27]=[N:28][N:29](C(OC(C)(C)C)=O)[CH:30]=2)O1.C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+]>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[NH:28]1[CH:27]=[C:26]([C:2]2[CH:3]=[C:4]([C@H:8]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])[CH3:9])[CH:5]=[CH:6][CH:7]=2)[CH:30]=[N:29]1
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참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 16217654tert-butyl 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylateHCID 679596071,1-Dimethylethyl N-[(1R)-1-(3-bromophenyl)ethyl]carbamate

생성물 1

HCID 89862967HCID 89862967, 화합물수율 74.6%

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

To a degassed solution of Intermediate 11A (3.00 g, 9.99 mmol), tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylate (4.410 g, 14.99 mmol) and potassium carbonate (4.14 g, 30.0 mmol) in dioxane (20 mL)/water (8 mL) was added Tetrakis (0.577 g, 0.500 mmol). The vial was purged with argon, sealed and stirred at 90° C. for 16 h. Another 20% of tetrakis and boronic ester were added and the reaction mixture was degassed and heated at 90° C. for 24 h. The reaction was cooled down to rt and NaOH (14.99 mL, 14.99 mmol) was added and the reaction was stirred at 50° C. for 5 h. The mixture was partitioned between EtOAc and water. The organic layer was separated. The aqueous phase was extracted with EtOAc, and the combined organic layers were dried over MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography over 120 g of silica gel (15 min gradient, with 0-100% ethyl acetate in hexanes) to afford Intermediate 11B (2.14 g, 7.45 mmol, 74.5% yield) as a white solid. LCMS=1.86 min [M+1]=288.2 (Method B).

후처리

  1. customThe vial was purged with argon
  2. customsealed
  3. additionAnother 20% of tetrakis and boronic ester were added
  4. customthe reaction mixture was degassed
  5. temperatureheated at 90° C. for 24 h
  6. temperatureThe reaction was cooled down to rt
  7. stirringthe reaction was stirred at 50° C. for 5 h
  8. customThe mixture was partitioned between EtOAc and water
  9. customThe organic layer was separated
  10. extractionThe aqueous phase was extracted with EtOAc
  11. dry with materialthe combined organic layers were dried over MgSO4
  12. concentrationconcentrated in vacuo
  13. customThe crude material was purified by flash chromatography over 120 g of silica gel (15 min gradient, with 0-100% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-a85c802e14af48c6b30dc99c66f368e1
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394260B2

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