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Methanol → 1-[5-(2-cyanopropan-2-yl)-2,3-dihydro-1H-inden-1-yl]-3-(1H-indazol-4-yl)urea

HRID 656458
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Reaktionsgleichung

Reaktionsgleichung von HRID 656458
COC([N:5]1[C:13]2[C:8](=[C:9]([NH:14][C:15]([O:17]N3C(=O)CCC3=O)=O)[CH:10]=[CH:11][CH:12]=2)[CH:7]=[N:6]1)=O.[NH2:25][CH:26]1[C:34]2[C:29](=[CH:30][C:31]([C:35]([CH3:39])([CH3:38])[C:36]#[N:37])=[CH:32][CH:33]=2)[CH2:28][CH2:27]1.CCN(C(C)C)C(C)C.CO>CN(C=O)C.O>[C:36]([C:35]([C:31]1[CH:30]=[C:29]2[C:34](=[CH:33][CH:32]=1)[CH:26]([NH:25][C:15]([NH:14][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]3[C:8]=1[CH:7]=[N:6][NH:5]3)=[O:17])[CH2:27][CH2:28]2)([CH3:39])[CH3:38])#[N:37]
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Komponenten

7

Edukt 4

HCID 887MethanolHCID 81531DiisopropylethylamineHCID 11313556methyl 4-({[(2,5-dioxo-1-pyrrolidinyl)oxy]carbonyl}amino)-1H-indazole-1-carboxylateHCID 671892902-(1-Aminoindan-5-yl)-2-methylpropionitrile

Produkt 1

HCID 671873051-[5-(2-cyanopropan-2-yl)-2,3-dihydro-1H-inden-1-yl]-3-(1H-indazol-4-yl)ureaAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel3×HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

4-(2,5-Dioxopyrrolidin-1-yl-oxycarbonylamino)-indazole-1-carboxylic acid methyl ester (3.31 g, 9.96 mmol) was added to a solution of 2-(1-aminoindan-5-yl)-2-methylpropionitrile (2.09 g, 10.5 mmol) and DIPEA (1.8 mL, 10.3 mmol) in DMF (40 mL) under nitrogen atmosphere at ambient temperature. After 1 hour the reaction solution was diluted with water (200 mL), the resulting white precipitate was filtered off, washed with water and air-dried. The wet cake was added to a solution of methanol (100 mL), water (3 mL) and TEA (2.8 mL, 20.1 mmol). The mixture was refluxed for 30 minutes, cooled the solution to room temperature, diluted with water (500 mL), collected the white precipitate by filtration, rinsed with water and air-dried. The wet cake was vacuum dried to constant weight, yielding 1-[5-(cyano-isopropyl)-indan-1-yl]-3-(1H-indazol-4-yl)-urea (3.32 g, 93%) as a white solid. MS (ESI) m/z: 360.07 [M+H]+. 1H NMR (DMSO-d6) δ: 1.69 (s, 6H), 1.87 (m, 1H), 2.47 (m, 1H), 2.89 (m, 1H), 2.98 (m, 1H), 5.19 (q, 1H), 6.73 (d, 1H), 7.08 (d, 1H), 7.22 (t, 1H), 7.39 (s, 2H), 7.44 (s, 1H), 7.66 (d, 1H), 8.04 (s, 1H), 8.59 (s, 1H), 13.00 (s, 1H). Anal Calcd for C21H21N5O.0.4H2O: C, 68.80; H, 5.99; N, 19.10. Found: C, 68.94; H, 5.72; N, 18.95.

Aufarbeitung

  1. filtrationthe resulting white precipitate was filtered off
  2. washwashed with water
  3. customair-dried
  4. temperatureThe mixture was refluxed for 30 minutes
  5. customcollected the white precipitate
  6. filtrationby filtration
  7. washrinsed with water
  8. customair-dried
  9. customdried to constant weight

Quellen und Nachweise

ORD-Eintrag
ord-c630279ec23e4cfbb11208579c642f8b
Quelldatensatz
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08071762B2

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