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Acetic Acid → HCID 178514862, 화합물

HRID 605003
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HRID 605003 반응식
Cl.Cl.[NH:3]1[CH2:8][CH2:7][CH:6]([C:9]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=3)[NH:11][N:10]=2)[CH2:5][CH2:4]1.[CH3:20][N:21]1[CH:30]=[CH:29][C:28]2[N:27]=[C:26]([C:31]3[CH:38]=[CH:37][C:34](C=O)=[CH:33][CH:32]=3)[C:25]([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)=[CH:24][C:23]=2[C:22]1=[O:45].C(N(CC)CC)C.[C:53](O)(=[O:55])C.[C:57](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>CN(C=O)C>[OH:55][CH2:53][CH2:20][N:21]1[CH:30]=[CH:29][C:28]2[N:27]=[C:26]([C:31]3[CH:38]=[CH:37][C:34]([CH2:57][N:3]4[CH2:8][CH2:7][CH:6]([C:9]5[N:13]=[C:12]([C:14]6[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=6)[NH:11][N:10]=5)[CH2:5][CH2:4]4)=[CH:33][CH:32]=3)[C:25]([C:39]3[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=3)=[CH:24][C:23]=2[C:22]1=[O:45]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 8471TriethylamineHCID 5049666Sodium triacetoxyborohydride2회HCID 866249424-(6-Methyl-5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehydeHCID 1784785342-(5-Piperidin-4-yl-4h-1,2,4-triazol-3-yl)-pyridine dihydrochloride

생성물 1

HCID 178514862
HCID 178514862, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-(3-piperidin-4-yl-1H-1,2,4-triazol-5-yl)pyridine dihydro-chloride (21 mg, 0.07 mmol) and 4-(6-methyl-5-oxo-3-phenyl-5,6-dihydro-1,6-naphthyridin-2-yl)benzaldehyde (17 mg, 0.046 mmol) in dry DMF (1.0 mL) was added triethyl-amine (25 mL, 0.18 mmol). After stirring for 10 minutes acetic acid (30 μL, 0.53 mmol) was added and the mixture was stirred at room temperature over night. Then sodium triacetoxy borohydride (17 mg, 0.08 mmol) was added in one portion. After monitoring by LC/MS it was determined the reaction was not complete and additional sodium triacetoxy borohydride (5 mg, 0.02 mmol)) were added and the reaction was stirred over night. This reaction mixture was concentrated to a smaller volume and adsorbed on silica gel and purified by column chromatography eluting with 20-100% ethyl acetate and then 0.5-9% methanol/ethyl acetate (sat'd NH3). The appropriate fractions were combined and the solvents removed in vacuo. The residue was triturated with diethyl ether to give pure title compound as a pale yellow solid. 1H NMR (500 MHz, CDCl3): δ 8.69 (1H, s), 8.64 (1H, d, J=4.4 Hz), 8.14 (1H, d, J=7.5 Hz), 7.83 (1H, t, J=7.5 Hz), 7.35-7.41 (5H, m), 7.21-7.28 (6H, m), 6.89 (1H, d, J=7.6 Hz), 4.24 (2H, t, J=4.8 Hz), 4.04 (2H, t, J=4.6 Hz), 3.58 (2H, vbr s), 3.00 (2H, vbr s), 2.86 (1H, m), 2.02-2.17 (4H, m). m/e (m+1): 584.1, 292.7 [(m+2)/2].

후처리

  1. additionwas added
  2. stirringthe reaction was stirred over night
  3. concentrationThis reaction mixture was concentrated to a smaller volume
  4. custompurified by column chromatography
  5. washeluting with 20-100% ethyl acetate
  6. customthe solvents removed in vacuo
  7. customThe residue was triturated with diethyl ether

출처 및 근거

ORD 기록
ord-743f26b9c78743699ffafaa9d9b7951d
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07910561B2

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