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Phosphoric Acid → 1-(2-(Tert-butoxy)pyridin-4-yl)-4-chloro-5-phenylphthalazine

HRID 593716
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HRID 593716 반응식
Cl[C:2]1[C:11]2[C:6](=[C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:8]=[CH:9][CH:10]=2)[C:5]([Cl:18])=[N:4][N:3]=1.[C:19]([O:23][C:24]1[CH:29]=[C:28](B2OC(C)(C)C(C)(C)O2)[CH:27]=[CH:26][N:25]=1)([CH3:22])([CH3:21])[CH3:20].P(=O)(O)(O)O.[K]>O1CCOCC1.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].F[B-](F)(F)F.C1([PH+](C2CCCCC2)C2CCCCC2)CCCCC1>[C:19]([O:23][C:24]1[CH:29]=[C:28]([C:2]2[C:11]3[C:6](=[C:7]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)[CH:8]=[CH:9][CH:10]=3)[C:5]([Cl:18])=[N:4][N:3]=2)[CH:27]=[CH:26][N:25]=1)([CH3:22])([CH3:20])[CH3:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 1004Phosphoric AcidHCID 5462222PotassiumHCID 457859932-(tert-Butoxy)-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridineHCID 904244121,4-Dichloro-5-phenylphthalazine

생성물 1

HCID 904241491-(2-(Tert-butoxy)pyridin-4-yl)-4-chloro-5-phenylphthalazine수율 70.8%

시약·촉매·용매 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 11710396Tricyclohexylphosphonium Tetrafluoroborate촉매
HCID 962Water용매2회
HCID 312751,4-Dioxane용매

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온도
95 °C

실험 절차

To a solution of 1,4-dichloro-5-phenylphthalazine (0.400 g, 1.45 mmol), 2-(tert-butoxy)-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (0.484 g, 1.75 mmol) in dioxane (20 mL) and water (2 mL) was added phosphoric acid, potassium salt (0.617 g, 2.91 mmol). The reaction mixture was purged with nitrogen gas for 30 min and then Pd2(dba)3 (0.013 g, 0.015 mmol) was added followed by tricyclohexylphosphonium tetrafluoroborate (11 mg, 0.029 mmol). The purging was continued for a further 15 min and the reaction mixture heated to 95° C. for 12 h. The reaction mixture was diluted with water (50 mL) and extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The resulting residue was purified by flash chromatography using Combiflash Isco (REDISEP®, SiO2, 12 g, 0-30% ethyl acetate/petroleum ether) to get 1-(2-(tert-butoxy)pyridin-4-yl)-4-chloro-5-phenylphthalazine (0.400 g, 33.2%) as a brown solid. LCMS (Condition 11): retention time 1.22 min, [M+1]=390.2. 1H NMR (400 MHz, DMSO-d6) δ 1.70 (s, 9 H), 6.84 (br s, 1 H), 7.05 (dd, J=1.2 Hz, J=5.2 Hz, 1 H), 7.36-7.44 (m, 2 H), 7.47-7.51 (m, 3 H), 8.06 (dd, J=1.2 Hz, J=7.6 Hz, 1 H), 8.15 (dd, J=0.8 Hz, J=4.8 Hz, 1 H), 8.26 (dd, J=7.2 Hz, J=8.0 Hz, 1 H), 8.47 (d, J=1.2 Hz, J=8.4 Hz, 1 H).

후처리

  1. customThe reaction mixture was purged with nitrogen gas for 30 min
  2. extractionextracted with ethyl acetate (3×50 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-93214ca7b7ca41e6ac298f1c052fe855
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242966B2

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