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Trifluoroacetic acid → HCID 58118717, 화합물

HRID 1866668
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HRID 1866668 반응식
[F:1][C:2]1[CH:3]=[C:4]([C@H:9]2[N:14](C(OC(C)(C)C)=O)[C:13](=[O:22])[C:12]([CH2:25][CH3:26])([CH2:23][CH3:24])[CH2:11][CH2:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([C@H:9]2[NH:14][C:13](=[O:22])[C:12]([CH2:25][CH3:26])([CH2:23][CH3:24])[CH2:11][CH2:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66864622HCID 66864622, 화합물

생성물 1

HCID 58118717HCID 58118717, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl (6S)-6-(3,5-difluorophenyl)-3,3-diethylpiperidin-2-one-1-carboxylate from Step D (1.22 g, 3.32 mmol) in CH2Cl2 (7 mL) at ambient temperature was added TFA (3 mL). After stirring for 1.5 h, the reaction mixture was concentrated in vacuo. The residue was partitioned between CH2Cl2 (30 mL) and saturated NaHCO3 (30 mL). The layers were separated and the aqueous layer was further extracted with CH2Cl2 (2×30 mL). The combined organics were dried over sodium sulfate, filtered and then concentrated in vacuo to provide the title compound, which could be used without further purification. MS: m/z=268 (M+1).

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customThe residue was partitioned between CH2Cl2 (30 mL) and saturated NaHCO3 (30 mL)
  3. customThe layers were separated
  4. extractionthe aqueous layer was further extracted with CH2Cl2 (2×30 mL)
  5. dry with materialThe combined organics were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-71a6ea55c3a446d382539158fc8246a2
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07629338B2

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