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Trifluoroacetic acid → 4-(3,4-Dichloro-phenyl)-3-methyl-1-(3-piperidin-1-yl-propyl)-piperazin-2-one

HRID 1096273
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HRID 1096273 반응식
FC(F)(F)C(O)=O.[Cl:8][C:9]1[CH:10]=[C:11]([NH:16][CH:17]([CH3:36])[C:18]([N:20]([CH2:30][CH:31](OC)OC)[CH2:21][CH2:22][CH2:23][N:24]2[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)=[O:19])[CH:12]=[CH:13][C:14]=1[Cl:15].C([SiH](CC)CC)C.C(N(CC)CC)C>C(Cl)Cl>[Cl:8][C:9]1[CH:10]=[C:11]([N:16]2[CH2:31][CH2:30][N:20]([CH2:21][CH2:22][CH2:23][N:24]3[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]3)[C:18](=[O:19])[CH:17]2[CH3:36])[CH:12]=[CH:13][C:14]=1[Cl:15]
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참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 12052TriethylsilaneHCID 667831682-(3,4-Dichloro-phenylamino)-N-(2,2-dimethoxy-ethyl)-N-(3-piperidin-1-yl-propyl)-propionamide

생성물 1

HCID 591592554-(3,4-Dichloro-phenyl)-3-methyl-1-(3-piperidin-1-yl-propyl)-piperazin-2-one수율 71.5%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

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온도
0 °C

실험 절차

Trifluoroacetic acid (1.15 g, 10.1 mmol) was added to a solution of 2-(3,4-dichloro-phenylamino)-N-(2,2-dimethoxy-ethyl)-N-(3-piperidin-1-yl-propyl)-propionamide (300 mg, 0.67 mmol) in CH2Cl2 (6 mL) at 0° C. After 30 min the ice bath was removed, then after 1 h triethylsilane (391 mg, 3.36 mmol) was added. After 16 h the reaction mixture was cooled to 0° C. and treated with triethylamine, then after 15 min partitioned between CH2Cl2 and sat. aq. NaHCO3 solution. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (IST Isolute® Flash NH2; EtOAc) afforded the title compound (184 mg, 71%). Yellow oil, MS: 384.2 (M+H)+.

후처리

  1. customAfter 30 min the ice bath was removed
  2. customafter 15 min partitioned between CH2Cl2 and sat. aq. NaHCO3 solution
  3. washThe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-a56f53edeb644ad0a47576be96b2d9f1
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08138175B2

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