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Water → 6-[5-(2,2,2-Trifluoro-1-hydroxy-1-methyl-ethyl)-3-pyridyl]-3,4-dihydro-2H-1,8-naphthyridine-1-carboxamide

HRID 712680
Notes
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Reaction equation

HRID 712680 reaction equation
CC1(C)C(C)(C)OB([C:9]2[CH:10]=[C:11]3[C:16](=[N:17][CH:18]=2)[N:15]([C:19]([NH2:21])=[O:20])[CH2:14][CH2:13][CH2:12]3)O1.Br[C:24]1[CH:25]=[C:26]([C:30]([OH:36])([CH3:35])[C:31]([F:34])([F:33])[F:32])[CH:27]=[N:28][CH:29]=1.C([O-])([O-])=O.[Na+].[Na+].O>O1CCOCC1>[F:34][C:31]([F:32])([F:33])[C:30]([C:26]1[CH:25]=[C:24]([C:9]2[CH:10]=[C:11]3[C:16](=[N:17][CH:18]=2)[N:15]([C:19]([NH2:21])=[O:20])[CH2:14][CH2:13][CH2:12]3)[CH:29]=[N:28][CH:27]=1)([OH:36])[CH3:35]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 666852642-(5-Bromopyridin-3-yl)-1,1,1-trifluoropropan-2-olHCID 1231626313,4-Dihydro-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,8-naphthyridine-1(2h)-carboxamide

Product 1

HCID 1176675706-[5-(2,2,2-Trifluoro-1-hydroxy-1-methyl-ethyl)-3-pyridyl]-3,4-dihydro-2H-1,8-naphthyridine-1-carboxamide

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
90 °C

Procedure

In a sealed tube which contains the crude 6-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-3,4-dihydro-2H-[1,8]naphthyridine-1-carboxylic acid amide (generated according to the procedure for Step 3 of Example 16 in 5 ml 1,4-dioxane, 0.78 mmol) is added 2-(5-bromo-pyridin-3-yl)-1,1,1-trifluoro-propan-2-ol (253 mg, 0.94 mmol.), Na2CO3 (166 mg, 1.56 mmol) and water (1.0 ml). The mixture is bubbled with Ar for 5 min. Then PdCl2(DPPF) DCM complex (64 mg, 0.078 mmol) is added. The mixture is then bubbled with Ar for 5 min. The cap is sealed and the mixture is heated at 90° C. in oil bath for 1 h and then is cooled to room temperature. The reaction mixture is filtered through diatomaceous earth and washed with DCM. The filtrate is partitioned between water and DCM. The aqueous phase is extracted with DCM. The combined DCM phases are concentrated. The crude is separated by flash silica gel column (EtOAc/heptane 0 to 100% gradient, then 100%). The fractions which contain the desired product are combined, concentrated and further purified by C-18 prep HPLC (MeCN with 0.1% TFA/Water with 0.1% TFA, 20 ml/min, 0 to 65% gradient over 10 min run). The desired fractions are combined and basified by 1N Na2CO3 to pH=10, and is extracted by DCM. The DCM phases are combined and concentrated under vacuum to obtain 69 mg of the title compound.

Workup

  1. customIn a sealed tube which contains
  2. customThe mixture is bubbled with Ar for 5 min
  3. additionThen PdCl2(DPPF) DCM complex (64 mg, 0.078 mmol) is added
  4. customThe mixture is then bubbled with Ar for 5 min
  5. customThe cap is sealed
  6. temperatureis cooled to room temperature
  7. filtrationThe reaction mixture is filtered through diatomaceous earth
  8. washwashed with DCM
  9. customThe filtrate is partitioned between water and DCM
  10. extractionThe aqueous phase is extracted with DCM
  11. concentrationThe combined DCM phases are concentrated
  12. customThe crude is separated by flash silica gel column (EtOAc/heptane 0 to 100% gradient
  13. concentrationconcentrated
  14. customfurther purified by C-18 prep HPLC (MeCN with 0.1% TFA/Water with 0.1% TFA, 20 ml/min, 0 to 65% gradient over 10 min run)
  15. extractionis extracted by DCM
  16. concentrationconcentrated under vacuum

Sources & evidence

ORD record
ord-bb97b4a8fb0c42f89ebbaefd590f7126
Source dataset
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09181272B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes