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Sodium t-butoxide → Tert-butyl 3-(2-fluoro-4-(methylsulfonyl)phenylamino)-2-oxo-1,4'-bipiperidine-1'-carboxylate

HRID 407935
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HRID 407935 반응식
[NH2:1][C@H:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH:8]2[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]2)[C:3]1=[O:21].Br[C:23]1[CH:28]=[CH:27][C:26]([S:29]([CH3:32])(=[O:31])=[O:30])=[CH:25][C:24]=1[F:33].CC([O-])(C)C.[Na+]>C1(C)C=CC=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[F:33][C:24]1[CH:25]=[C:26]([S:29]([CH3:32])(=[O:31])=[O:30])[CH:27]=[CH:28][C:23]=1[NH:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([CH:8]2[CH2:9][CH2:10][N:11]([C:14]([O:16][C:17]([CH3:18])([CH3:20])[CH3:19])=[O:15])[CH2:12][CH2:13]2)[C:3]1=[O:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 23676156Sodium t-butoxideHCID 467389084-Bromo-3-fluorophenyl methyl sulphoneHCID 66802275(S)-tert-butyl 3-amino-2-oxo-1,4'-bipiperidine-1'-carboxylate

생성물 1

HCID 66802697Tert-butyl 3-(2-fluoro-4-(methylsulfonyl)phenylamino)-2-oxo-1,4'-bipiperidine-1'-carboxylate수율 106%

시약·촉매·용매 3

HCID 634876
Binap, (A+-)-
촉매
HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 1140Toluene용매

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온도
80 °C

실험 절차

(S)-tert-Butyl 3-amino-2-oxo-1,4′-bipiperidine-1′-carboxylate (Example 39, Steps A-C, 5.0 g, 17 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (1.0 g, 1.7 mmol), 1-bromo-2-fluoro-4-(methylsulfonyl)benzene (6.4 g, 25 mmol) and NaOtBu (1.9 g, 20 mmol) were dissolved in degassed toluene (100 mL). Pd2 dba3 (0.77 g, 0.84 mmol) was added and the reaction heated in an 80° C. oil bath for 5 hours. The reaction was concentrated and purified over silica gel (50-100% EtOAc in hexanes followed by 5% ammoniated methanol in CH2Cl2) to afford tert-butyl 3-(2-fluoro-4-(methylsulfonyl)phenylamino)-2-oxo-1,4′-bipiperidine-1′-carboxylate (8.4 g, 18 mmol, 106% yield) as yellow solid.

후처리

  1. concentrationThe reaction was concentrated
  2. custompurified over silica gel (50-100% EtOAc in hexanes followed by 5% ammoniated methanol in CH2Cl2)

출처 및 근거

ORD 기록
ord-4179f3243d2248b9a0443f98bb7f97a1
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08754226B2

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