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Acetic Acid → {2-[5-(1-Methyl-2-oxo-1,2,3,4-tetrahydro-quinolin-6-yl)-3,4-dihydro-2H-[1,7]naphthyridin-1-yl]-ethyl}-carbamic acid tert-butyl ester

HRID 530351
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HRID 530351 반응식
[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]3[CH:21]=[N:20][CH:19]=[C:18]4[C:13]=3[CH2:14][CH2:15][CH2:16][NH:17]4)=[CH:9][CH:10]=2)[CH2:5][CH2:4][C:3]1=[O:22].O=[CH:24][CH2:25][NH:26][C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30].C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>ClCCCl.C(Cl)Cl.C1COCC1>[C:29]([O:28][C:27](=[O:33])[NH:26][CH2:25][CH2:24][N:17]1[C:18]2[C:13](=[C:12]([C:8]3[CH:7]=[C:6]4[C:11](=[CH:10][CH:9]=3)[N:2]([CH3:1])[C:3](=[O:22])[CH2:4][CH2:5]4)[CH:21]=[N:20][CH:19]=2)[CH2:14][CH2:15][CH2:16]1)([CH3:32])([CH3:31])[CH3:30]
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참가 물질

9

반응물 5

HCID 176Acetic AcidHCID 516892Sodium BicarbonateHCID 4247255tert-butyl N-(2-oxoethyl)carbamateHCID 5049666Sodium triacetoxyborohydrideHCID 866799281-Methyl-6-(1,2,3,4-tetrahydro-1,7-naphthyridin-5-yl)-3,4-dihydroquinolin-2(1H)-one

생성물 1

HCID 71536484
{2-[5-(1-Methyl-2-oxo-1,2,3,4-tetrahydro-quinolin-6-yl)-3,4-dihydro-2H-[1,7]naphthyridin-1-yl]-ethyl}-carbamic acid tert-butyl ester
수율 24.2%

시약·촉매·용매 3

HCID 111,2-Dichloroethane용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-methyl-6-(1,2,3,4-tetrahydro-1,7-naphthyridin-5-yl)-3,4-dihydroquinolin-2(1H)-one (intermediate A-5, 0.1 g, 0.341 mmol) in DCE (3 mL)/THF (1.5 mL) were added tert-butyl 2-oxoethylcarbamate (0.081 g, 0.511 mmol), acetic acid (0.02 g, 0.341 mmol) and the reaction mixture was stirred at room temperature for 10 min. Then, sodium triacetoxyborohydride (0.144 g, 0.682 mmol) was added and stirring was continued at room temperature over night. Then, the mixture was diluted with DCM, poured into aq NaHCO3 and extracted with DCM (2×25 mL). Combined organics were washed with brine, dried over Na2SO4, filtered and evaporated to dryness. The residue was purified by reverse phase HPLC on a Gemini-NX column, eluting with a 20 to 98% MeOH—H2O (0.05% TEA) gradient to give the title compound (0.036 g, 24%) as a white foam. MS: 437.2 (M+H+).

후처리

  1. stirringstirring
  2. waitwas continued at room temperature over night
  3. extractionextracted with DCM (2×25 mL)
  4. washCombined organics were washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe residue was purified by reverse phase HPLC on a Gemini-NX column
  9. washeluting with a 20 to 98% MeOH—H2O (0.05% TEA) gradient

출처 및 근거

ORD 기록
ord-46c75fa127ee4202ba645e255413c4dd
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09353081B2

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