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Formaldehyde → HCID 70874784, 화합물

HRID 2208715
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HRID 2208715 반응식
[CH:1]1([N:6]([CH3:33])[C:7]2[C:8]([CH3:32])=[C:9]([CH:23]=[C:24]([C:26]3[CH2:27][CH2:28][NH:29][CH2:30][CH:31]=3)[CH:25]=2)[C:10]([NH:12][CH2:13][C:14]2[C:15](=[O:22])[NH:16][C:17]([CH3:21])=[CH:18][C:19]=2[CH3:20])=[O:11])[CH2:5][CH2:4][CH2:3][CH2:2]1.C=O.[C:36]([BH3-])#N.[Na+]>CO>[CH:1]1([N:6]([CH3:33])[C:7]2[C:8]([CH3:32])=[C:9]([CH:23]=[C:24]([C:26]3[CH2:27][CH2:28][N:29]([CH3:36])[CH2:30][CH:31]=3)[CH:25]=2)[C:10]([NH:12][CH2:13][C:14]2[C:15](=[O:22])[NH:16][C:17]([CH3:21])=[CH:18][C:19]=2[CH3:20])=[O:11])[CH2:2][CH2:3][CH2:4][CH2:5]1
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참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 5003444Sodium cyanoborohydrideHCID 70874367HCID 70874367, 화합물

생성물 1

HCID 70874784HCID 70874784, 화합물수율 63%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

3-(Cyclopentyl(methyl)amino)-N-((4,6-dimethyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-2-methyl-5-(1,2,3,6-tetrahydropyridin-4-yl)benzamide (0.100 g, 0.223 mmol) was dissolved in methanol (5 mL) and cooled to 0° C., formalin (0.067 g, 0.19 mL, 2.23 mmol) was added. Resulting reaction mass was stirred at same temperature for 30 minutes. Sodium cyanoborohydride (0.041 g, 0.66 mmol) was added to above reaction mass and stirred at room temperature for 4 h. After completion, solvent were removed under reduced pressure and water was added to the residue, extraction was carried out using DCM. Combined organic layers were dried, concentrated and purified by column chromatography to provide the desired compound (0.065 g, 63%): LCMS: 463.40 (M+1)+; HPLC: 98.79% (@ 254 nm) (Rt; 3.911; Method: Column: YMC ODS-A 150 mm×4.6 mm×5μ; Mobile Phase: A; 0.05% TFA in water/B; 0.05% TFA in acetonitrile; Inj. Vol: 10 μL, Col. Temp.: 30° C.; Flow rate: 1.4 mL/min.; Gradient: 5% B to 95% B in 8 min, Hold for 1.5 min, 9.51-12 min 5% B); 1H NMR (DMSO-d6, 400 MHz) δ 11.43 (s, 1H), 8.04 (t, 1H, J=4.8 Hz), 7.17 (s, 1H), 6.95 (s, 1H), 6.07 (s, 1H), 5.85 (s, 1H), 4.25 (d, 2H, J=4.8 Hz), 3.45 (m, 1H), 2.98 (bs, 2H), 2.53 (m, 2H), 2.42 (bs, 2H), 2.26 (s, 3H), 2.18 (s, 3H), 2.17 (s, 3H), 2.10 (s, 3H), 1.67 (m, 2H), 1.59 (m, 2H), 1.49 (m, 2H), 1.40 (m, 2H).

후처리

  1. customResulting
  2. customreaction mass
  3. stirringstirred at room temperature for 4 h
  4. customAfter completion, solvent were removed under reduced pressure and water
  5. additionwas added to the residue, extraction
  6. customCombined organic layers were dried
  7. concentrationconcentrated
  8. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-e0dec9bc92d8448d8232fc08ac9d1bd8
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376422B2

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