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Cyclohexanone → HCID 86603668, 화합물

HRID 2376047
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HRID 2376047 반응식
Cl.Cl.[NH:3]1[CH2:8][CH2:7][CH2:6][C@@H:5]([NH:9][C:10]2[N:11]=[CH:12][C:13](/[CH:16]=[CH:17]/[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[N:14][CH:15]=2)[CH2:4]1.C(N(C(C)C)CC)(C)C.[C:32]1(=O)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1.[Na].C(=O)(O)[O-].[Na+]>ClCCCl>[CH:32]1([N:3]2[CH2:8][CH2:7][CH2:6][C@@H:5]([NH:9][C:10]3[N:11]=[CH:12][C:13](/[CH:16]=[CH:17]/[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[N:14][CH:15]=3)[CH2:4]2)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 7967CyclohexanoneHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 5360545SodiumHCID 86603669ethyl (2E)-3-{5-[(3R)-3-piperidinylamino]-2-pyrazinyl)acrylate dihydrochloride

생성물 1

HCID 86603668HCID 86603668, 화합물수율 76.3%

시약·촉매·용매

1
HCID 111,2-Dichloroethane용매

실험 절차

To a solution of ethyl (2E)-3-{5-[(3R)-3-piperidinylamino]-2-pyrazinyl)acrylate dihydrochloride (300 mg) in 1,2-dichloroethane (5 mL) were added diisopropylethylamine (222 mg) and cyclohexanone (93 mg), and the mixture was stirred at ambient temperature for 5 min. To the mixture was added sodium triacetoxybrohydryde (364 mg) and stirred for 4 hrs, and resulting mixture was poured into saturated sodium bicarbonate solution, and extracted with chloroform. The organic layer was washed with water, and brine, and dried over magnesium sulfate. The solvent was removed in vacuo and the residue was purified by preparative thin layer chromatography (chloroform-MeOH=10-1) to give ethyl (2E)-3-(5-{[(3R)-1-cyclohexyl-3-piperidinyl]amino}-2-pyrazinyl)acrylate (235 mg) as an amorphous powder.

후처리

  1. stirringstirred for 4 hrs
  2. customresulting mixture
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with water, and brine
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed in vacuo
  7. customthe residue was purified by preparative thin layer chromatography (chloroform-MeOH=10-1)

출처 및 근거

ORD 기록
ord-31a8e51b4c09483694acc472ba6e0a2e
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07465731B2

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