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Trifluoroacetic acid → 4-[(4-{4-[(1E)-3-hydroxyprop-1-en-1-yl]phenyl}pyrimidin-2-yl)amino]benzenesulfonamide

HRID 1715694
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HRID 1715694 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([S:21]([NH2:24])(=[O:23])=[O:22])=[CH:17][CH:16]=3)[N:9]=2)=[CH:4][CH:3]=1.C([Si](C)(C)[O:30][CH2:31]/[CH:32]=[CH:33]/B1OC(C)(C)C(C)(C)O1)(C)(C)C.C(=O)([O-])[O-].[K+].[K+].FC(F)(F)C(O)=O>C1(C)C=CC=CC=1.O.C(O)C>[OH:30][CH2:31]/[CH:32]=[CH:33]/[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]3[CH:20]=[CH:19][C:18]([S:21]([NH2:24])(=[O:23])=[O:22])=[CH:17][CH:16]=3)[N:9]=2)=[CH:4][CH:3]=1
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참가 물질

8

반응물 4

HCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 10968526(E)-3-(tert-Butyldimethylsilyloxy)propene-1-yl-boronic acid pinacol esterHCID 574467974-{[4-(4-Bromophenyl)pyrimidin-2-yl]amino}benzenesulfonamide

생성물 1

HCID 114946764-[(4-{4-[(1E)-3-hydroxyprop-1-en-1-yl]phenyl}pyrimidin-2-yl)amino]benzenesulfonamide수율 30.5%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 1140Toluene용매

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온도
85 °C

실험 절차

A flask is charged with 4-{[4-(4-bromophenyl)pyrimidin-2-yl]amino}benzenesulfonamide (0.681 g, 1.68 mmol), tert-butyl(dimethyl){[(2E)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)prop-2-en-1-yl]oxy}silane (1.00 g, 3.35 mmol), (Ph3)4Pd (0.194 g, 0.168 mmol), potassium carbonate (0.695 g, 5.03 mmol), ethanol (3.0 ml), water (3.0 ml), and toluene (25 ml). The reaction mixture is stirred at 85° C. for 4 h. The reaction mixture is cooled to room temperature, and trifluoroacetic acid (1.0 ml) is added. The reaction mixture is then stirred for 16 h at room temperature. The reaction mixture is concentrated and purified on preparative HPLC to yield 0.196 g of a yellow solid. MS (ESI) m/z 383.2; HRMS: calcd for C19H18N4O3S+H+, 383.11724; found (ESI-FTMS, [M+H]1+), 383.11752.

후처리

  1. temperatureThe reaction mixture is cooled to room temperature
  2. stirringThe reaction mixture is then stirred for 16 h at room temperature
  3. concentrationThe reaction mixture is concentrated
  4. custompurified on preparative HPLC

출처 및 근거

ORD 기록
ord-2b9f74d9422d40adb5ebc5ed4079b739
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07799915B2

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