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Benzyl piperazine-1-carboxylate → Benzyl 4-(2-(benzyloxy)pyridin-3-yl)piperazine-1-carboxylate

HRID 1804619
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HRID 1804619 반응식
C1(P(C2CCCCC2)C2C=CC=CC=2C2C(N(C)C)=CC=CC=2)CCCCC1.[CH2:29]([O:36][C:37]1[C:42](Br)=[CH:41][CH:40]=[CH:39][N:38]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.[N:44]1([C:50]([O:52][CH2:53][C:54]2[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=2)=[O:51])[CH2:49][CH2:48][NH:47][CH2:46][CH2:45]1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.O.C1(/C=C/C(=O)/C=C/C2C=CC=CC=2)C=CC=CC=1.[Pd]>[CH2:29]([O:36][C:37]1[C:42]([N:47]2[CH2:46][CH2:45][N:44]([C:50]([O:52][CH2:53][C:54]3[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=3)=[O:51])[CH2:49][CH2:48]2)=[CH:41][CH:40]=[CH:39][N:38]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
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참가 물질

8

반응물 4

HCID 643495Benzyl piperazine-1-carboxylateHCID 27342172-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenylHCID 147124562-Benzyloxy-3-bromopyridineHCID 23676156Sodium t-butoxide

생성물 1

HCID 67060675Benzyl 4-(2-(benzyloxy)pyridin-3-yl)piperazine-1-carboxylate수율 55%

시약·촉매·용매 3

HCID 15673654
(1E,4E)-1,5-diphenyl-1,4-pentadien-3-one palladium
촉매
HCID 962Water용매
HCID 1140Toluene용매

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온도
80 °C

실험 절차

To a stirred suspension of 0.011 g (0.012 mmol) of (1E,4E)-1,5-diphenylpenta-1,4-dien-3-one-palladium (3:2) in 3 mL of anhydrous toluene under an atmosphere of nitrogen was added 0.015 g (0.037 mmol) of 2′-(dicyclohexylphosphino)-N,N-dimethylbiphenyl-2-amine and the resulting mixture was allowed to stir for 20 min. Next, 0.11 g (0.41 mmol) of 2-(benzyloxy)-3-bromopyridine was added followed by 0.11 g (0.49 mmol) of benzyl piperazine-1-carboxylate and 0.059 g (0.61 mmol) of sodium tert-butoxide. The resulting mixture was then heated to 80° C. overnight. After cooling to ambient temperature, the reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with water then brine, dried over magnesium sulfate and evaporated to dryness in vacuo. The residue was purified by silica gel chromatography eluting with a 0-100% acetone in hexanes gradient to afford the title compound as clear gum (0.090 g, 55%). 1H-NMR (500 MHz, CDCl3) δ 7.84 (dd, J=4.9, 1.6 Hz, 1H), 7.47-7.29 (m, 10H), 7.09 (dd, J=7.5, 1.6 Hz, 1H), 6.87 (dd, J=7.5, 4.9 Hz, 1H), 5.46 (s, 2H), 5.16 (s, 2H), 3.67-3.65 (m, 4H), 3.07 (br s, 4H). LC-MS: m/z (ES) 404.0 (MH)+.

후처리

  1. temperatureAfter cooling to ambient temperature
  2. extractionextracted with ethyl acetate
  3. washThe combined organic layers were washed with water
  4. dry with materialbrine, dried over magnesium sulfate
  5. customevaporated to dryness in vacuo
  6. customThe residue was purified by silica gel chromatography
  7. washeluting with a 0-100% acetone in hexanes gradient

출처 및 근거

ORD 기록
ord-c69d606ce85b4564ae29aa1d539c9d58
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354403B2

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