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Triethylamine → {3-[1-(3-Benzyl-4-oxo-3,4-dihydro-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-propylamino]-propyl}-carbamic acid tert-butyl ester

HRID 1795945
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HRID 1795945 반응식
[CH2:1]([N:8]1[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][N:11]2[N:10]=[C:9]1[CH:18](O)[CH2:19][CH3:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.S([O-])(=O)(=O)C.[C:39]([NH:46][CH2:47][CH2:48][CH2:49][NH2:50])([O:41][C:42]([CH3:45])([CH3:44])[CH3:43])=[O:40]>C(Cl)Cl.C([O-])(O)=O.[Na+].CCOC(C)=O.CN1C(=O)CCC1.O>[C:42]([O:41][C:39](=[O:40])[NH:46][CH2:47][CH2:48][CH2:49][NH:50][CH:18]([C:9]1[N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][N:11]2[N:10]=1)[CH2:19][CH3:20])([CH3:45])([CH3:43])[CH3:44]
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참가 물질

11

반응물 5

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 85257MethanesulfonateHCID 2735700tert-Butyl (3-aminopropyl)carbamateHCID 22180024(+/-)-3-Benzyl-2-(1-hydroxy-propyl)-3H-pyrrolo[2,1-f][1,2,4]triazin-4-one

생성물 1

HCID 21025743
{3-[1-(3-Benzyl-4-oxo-3,4-dihydro-pyrrolo[2,1-f][1,2,4]triazin-2-yl)-propylamino]-propyl}-carbamic acid tert-butyl ester
수율 61%

시약·촉매·용매 5

HCID 962Water용매HCID 6344Dichloromethane용매2회HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매HCID 516892Sodium Bicarbonate용매

실험 절차

To a solution of (±)-3-benzyl-2-(1-hydroxy-propyl)-3H-pyrrolo[2,1-f][1,2,4]triazin-4-one (0.70 g, 2.47 mmol) in methylene chloride (20 mL) at 0° C. was added triethylamine (517 μL, 3.71 mmol) followed by methanesulfonyl chloride (290 μL, 3.71 mmol). The reaction was stirred at room temperature for 45 min and was then diluted methylene chloride (10 mL) and water (10 mL). The layers were separated and the aqueous layer was extracted with methylene chloride (10 mL). The combined organic extracts were washed with brine (10 mL), dried over anhydrous MgSO4, and concentrated in vacuo. The crude mesylate was treated with N-BOC-1,3-diaminopropane (Fluka, 1.29 g, 7.41 mmol) and NMP (20 mL) at 75° C. for 14 h. After cooling to room temperature, the reaction was diluted with saturated NaHCO3 solution (30 mL) and EtOAc (30 mL). The layers were separated and the aqueous layer was extracted with EtOAc (2×30 mL). The combined organic extracts were washed with 10% LiCl solution (30 mL), dried over anhydrous MgSO4, and concentrated in vacuo. Purification of the crude product by flash column chromatography (SiO2, EtOAc/Hexane 1:1) gave the title compound as a colorless viscous oil (610 mg, 61%): 1H NMR (CDCl3) δ 7.25 (m, 6H), 7.01 (m, 1H), 6.47 (m, 1H), 5.66 (d, 1H, J=16.2 Hz), 5.04 (brs, 1H), 4.85 (d, 1H, J=16.1 Hz), 3.48 (m, 1H), 2.91 (m, 2H), 2.42 (m, 1H), 1.96 (m, 1H), 1.64 (m, 2H), 1.34 (s, 9H), 1.28 (m, 2H), 0.86 (t, 3H, J=7.28 Hz); 13C NMR (CDCl3) δ 156.3, 155.7, 151.6, 137.1, 129.4, 128.1, 126.8, 121.3, 118.4, 111.2, 109.2, 79.3, 59.9, 45.8, 44.5, 39.7, 29.8, 28.8, 28.6, 11.2; MS (ESI+) 440.29 (M++H).

후처리

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted with methylene chloride (10 mL)
  3. washThe combined organic extracts were washed with brine (10 mL)
  4. dry with materialdried over anhydrous MgSO4
  5. concentrationconcentrated in vacuo
  6. temperatureAfter cooling to room temperature
  7. customThe layers were separated
  8. extractionthe aqueous layer was extracted with EtOAc (2×30 mL)
  9. washThe combined organic extracts were washed with 10% LiCl solution (30 mL)
  10. dry with materialdried over anhydrous MgSO4
  11. concentrationconcentrated in vacuo
  12. customPurification of the crude product by flash column chromatography (SiO2, EtOAc/Hexane 1:1)

출처 및 근거

ORD 기록
ord-3493b9ba56254648a70eb40fe43da435
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030118B2

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