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Potassium Phosphate, Tribasic → HCID 57454141, 화합물

HRID 546948
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HRID 546948 반응식
C([Si](C)(C)[O:6][C:7]([C:42]([F:45])([F:44])[F:43])([C:38]([F:41])([F:40])[F:39])/[CH:8]=[CH:9]/[C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:21]2[CH:26]=[CH:25][C:24](B3OC(C)(C)C(C)(C)O3)=[C:23]([CH3:36])[CH:22]=2)([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:12][C:11]=1[CH3:37])(C)(C)C.[CH2:48]([O:50][C:51](=[O:60])[CH2:52][C:53]1[CH:54]=[N:55][C:56](Br)=[N:57][CH:58]=1)[CH3:49].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>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>[CH2:48]([O:50][C:51](=[O:60])[CH2:52][C:53]1[CH:54]=[N:55][C:56]([C:24]2[CH:25]=[CH:26][C:21]([C:16]([CH2:19][CH3:20])([C:13]3[CH:14]=[CH:15][C:10](/[CH:9]=[CH:8]/[C:7]([OH:6])([C:42]([F:44])([F:45])[F:43])[C:38]([F:41])([F:40])[F:39])=[C:11]([CH3:37])[CH:12]=3)[CH2:17][CH3:18])=[CH:22][C:23]=2[CH3:36])=[N:57][CH:58]=1)[CH3:49]
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참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 57443494Ethyl 2-(2-bromopyrimidin-5-yl)acetateHCID 57709023HCID 57709023, 화합물

생성물 1

HCID 57454141HCID 57454141, 화합물수율 41%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 962
Water
용매

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온도
95.5 °C

실험 절차

Degassed N,N-dimethylformamide (0.32 mL) was added to 2-[4-(1-{4-[(E)-3-(t-butyl-dimethyl-silanyloxy)-4,4,4-trifluoro-3-trifluoromethyl-1-butenyl]-3-methyl-phenyl}-1-ethyl-propyl)-2-methyl-phenyl]-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (Example 77-(1); 35.8 mg, 0.0523 mmol), 2-bromopyrimidine-5-acetic acid ethyl ester (Example 43-(3); 37.3 mg, 0.152 mmol), tetrakis(triphenylphosphine)palladium (0) (29.8 mg, 0.0258 mmol) and potassium phosphate (48.7 mg, 0.229 mmol). After replacement with nitrogen, the mixture was heated while stirring at an external temperature of 91 to 100° C. for 10 hours. Water was added to the reaction mixture, followed by extraction with diethyl ether. The extract was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=4/1) to give the title compound (13 mg, 41%).

후처리

  1. customDegassed N,N-dimethylformamide (0.32 mL)
  2. temperatureAfter replacement with nitrogen, the mixture was heated
  3. extractionfollowed by extraction with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-610b11214dc440febaf0223b2a15078a
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935688B2

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