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Iodoethane → ethyl 6-{[(3R)-1-benzyl-3-piperidinyl]amino}-5-chloronicotinate

HRID 226465
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HRID 226465 반응식
[Cl:1][C:2]1[C:3](Cl)=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].I[CH2:13][CH3:14].C([O-])([O-])=O.[K+].[K+].Cl.Cl.[CH2:23]([N:30]1[CH2:35][CH2:34][CH2:33][C@@H:32]([NH2:36])[CH2:31]1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CN(C=O)C>[CH2:23]([N:30]1[CH2:35][CH2:34][CH2:33][C@@H:32]([NH:36][C:3]2[C:2]([Cl:1])=[CH:10][C:6]([C:7]([O:9][CH2:13][CH3:14])=[O:8])=[CH:5][N:4]=2)[CH2:31]1)[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
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참가 물질

6

반응물 4

HCID 6340IodoethaneHCID 11430Potassium Carbonate2회HCID 2479875,6-Dichloronicotinic acidHCID 22831369(R)-1-benzyl-3-Aminopiperidine Dihydrochloride

생성물 1

HCID 68964359ethyl 6-{[(3R)-1-benzyl-3-piperidinyl]amino}-5-chloronicotinate수율 52%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

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온도
45 °C

실험 절차

To a solution of 5,6-dichloronicotinic acid (7.0, 35 mmol) in DMF were added iodoethane (6.0 g, 38.5 mmol) and K2CO3 (5.8 g, 42 mmol) at ambient temperature and the mixture was stirred at 45° C. for 5 hrs. To the reaction mixture were added (3R)-1-benzyl-3-piperidinamine dihydrochloride (10.1 g, 38.5 mmol) and K2CO3 (16.9 g, 122 mmol) and the reaction mixture was stirred at 90° C. for 18 hrs. The reaction mixture was evaporated in vacuo and the residue was partitioned between water and EtOAc. The organic layer was separated, washed water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (EtOAc-hexane/1-4˜1-3) to give ethyl 6-{[(3R)-1-benzyl-3-piperidinyl]amino}-5-chloronicotinate (6.75 g, 52%) as a powder.

후처리

  1. stirringthe reaction mixture was stirred at 90° C. for 18 hrs
  2. customThe reaction mixture was evaporated in vacuo
  3. customthe residue was partitioned between water and EtOAc
  4. customThe organic layer was separated
  5. washwashed water and brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated in vacuo
  8. customThe residue was purified by silica gel column chromatography (EtOAc-hexane/1-4˜1-3)

출처 및 근거

ORD 기록
ord-9ab467195a50421283683d60a06869e0
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07557127B2

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