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N-Boc-pyrrolidine → (R)-tert-butyl 2-(2-oxoindolin-4-yl)pyrrolidine-1-carboxylate

HRID 529136
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HRID 529136 반응식
C([Li])(CC)C.[N:6]1([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:10][CH2:9][CH2:8][CH2:7]1.Br[C:19]1[CH:27]=[CH:26][CH:25]=[C:24]2[C:20]=1[CH2:21][C:22](=[O:28])[NH:23]2.F[B-](F)(F)F.C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>CC(OC)(C)C.[Cl-].[Zn+2].[Cl-].C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CCOC(C)=O>[O:28]=[C:22]1[CH2:21][C:20]2[C:24](=[CH:25][CH:26]=[CH:27][C:19]=2[C@H:7]2[CH2:8][CH2:9][CH2:10][N:6]2[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[NH:23]1
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참가 물질

9

반응물 4

HCID 643455N-Boc-pyrrolidineHCID 27631904-bromo-2,3-dihydro-1H-indol-2-oneHCID 44558591Tri-t-butylphosphine fluoroborateHCID 178418400CID 53628100

생성물 1

HCID 69812735(R)-tert-butyl 2-(2-oxoindolin-4-yl)pyrrolidine-1-carboxylate수율 27%

시약·촉매·용매 4

HCID 167845
palladium(II) acetate
촉매
HCID 3007855Zincchloride촉매
HCID 8857Ethyl Acetate용매
HCID 15413tert-Butyl methyl ether용매

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온도
-78 °C

실험 절차

sec-Butyl lithium (25.3 mL, 35.4 mmol) was added into a solution of tert-butyl 1-pyrrolidinecarboxylate (6.2 mL, 35.4 mmol) and (−)-spartiene (8.29 g, 35.4 mmol) in MTBE (100 mL) at −78° C. The mixture was stirred for 1 hour at −78° C. Zinc chloride solution (35.4 mL, 35.4 mmol) was added, and the reaction was stirred for 15 minutes at −78° C. The reaction was allowed to warm up to room temperature. 4-Bromoindolin-2-one (5.00 g, 23.6 mmol), palladium (II) acetate (0.53 g, 2.4 mmol) and tri-tert-butylphosphine tetrafluoroborate (0.68 g, 2.4 mmol) was added into the reaction mixture. The reaction was stirred for 12 hours at room temperature. The reaction mixture was poured into EtOAc (200 mL), and the suspension was filtered with a pad of celite. The filtrate was concentrated, and the residue was purified by flash chromatography (silica gel eluted with 4:1 hexanes:ethyl acetate) to give (R)-tert-butyl 2-(2-oxoindolin-4-yl)pyrrolidine-1-carboxylate (1.9 g, 27%) as a solid. 1H NMR (CDCl3, 400 MHz) δ 7.80 (s, 1H), 7.10-7.20 (m, 1H), 6.75-6.82 (m, 1H), 6.62-6.78 (m, 1H), 4.65-4.93 (m, 1H), 3.34-3.73 (m, 4H), 2.20-2.40 (m, 1H), 1.84-2.00 (m, 2H), 1.68-1.83 (m, 1H), 1.45 (2, 4H), 1.14 (s, 5H). MS (APCI+) [M+H]+ 303.

후처리

  1. stirringthe reaction was stirred for 15 minutes at −78° C
  2. temperatureto warm up to room temperature
  3. stirringThe reaction was stirred for 12 hours at room temperature
  4. filtrationthe suspension was filtered with a pad of celite
  5. concentrationThe filtrate was concentrated
  6. customthe residue was purified by flash chromatography (silica gel eluted with 4:1 hexanes:ethyl acetate)

출처 및 근거

ORD 기록
ord-dcb387eb90b84d108a43c0e3b21a26fe
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346805B2

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