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Methanol → 1-(1H-Indazol-4-yl)-3-(4-piperidin-1-yl-indan-1-yl)-urea

HRID 2223414
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2223414
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.[N:25]1([C:31]2[CH:39]=[CH:38][CH:37]=[C:36]3[C:32]=2[CH2:33][CH2:34][CH:35]3[NH2:40])[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]1.CCN(C(C)C)C(C)C.CO>CN(C=O)C.O>[NH:5]1[C:13]2[C:8](=[C:9]([NH:14][C:15]([NH:40][CH:35]3[C:36]4[C:32](=[C:31]([N:25]5[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]5)[CH:39]=[CH:38][CH:37]=4)[CH2:33][CH2:34]3)=[O:17])[CH:10]=[CH:11][CH:12]=2)[CH:7]=[N:6]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 887MethanolHCID 81531DiisopropylethylamineHCID 11313556methyl 4-({[(2,5-dioxo-1-pyrrolidinyl)oxy]carbonyl}amino)-1H-indazole-1-carboxylateHCID 671879554-Piperidin-1-ylindan-1-ylamine

Produkt 1

HCID 112342231-(1H-Indazol-4-yl)-3-(4-piperidin-1-yl-indan-1-yl)-ureaAusbeute 93,4 %

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 962WaterLösungsmittel3×HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

4-(2,5-Dioxopyrrolidin-1-yl-oxycarbonylamino)-indazole-1-carboxylic acid methyl ester (5.57 g, 16.8 mmol) was added to a solution of 4-piperidin-1-ylindan-1-ylamine (3.81 g, 17.6 mmol) and DIPEA (3.0 mL, 17.2 mmol) in DMF (80 mL) under nitrogen atmosphere at ambient temperature. After 30 minutes the reaction solution was diluted with water (350 mL), the resulting beige precipitate was filtered off, washed with water and air-dried. The wet cake was added to a solution of methanol (200 mL), water (3 mL) and TEA (7.0 mL, 50.2 mmol). The mixture was refluxed for 90 minutes, cooled to room temperature, diluted with water (200 mL), collected the beige precipitate by filtration, rinsed with water and air-dried. The wet cake was vacuum dried to constant weight, yielding 1-(1H-indazol-4-yl)-3-(4-piperidin-1-ylindan-1-yl)-urea (5.89 g, 93%) as a beige solid. MS (ESI) m/z: 376.00 [M+H]+. 1H NMR (DMSO-d6) δ: 1.56 (m, 2H), 1.65 (m, 4H), 1.78 (m, 1H), 2.44 (m, 1H), 2.77 (m, 1H), 2.85 (m, 3H), 2.95 (m, 2H), 5.16 (q, 1H), 6.66 (d, 1H), 6.81 (d, 1H), 6.95 (d, 1H), 7.07 (d, 1H), 7.22 (m, 2H), 7.68 (d, 1H), 8.05 (s, 1H), 8.62 (s, 1H), 13.00 (s, 1H). Anal Calcd for C22H25N5O: C, 70.38; H, 6.71; N, 18.65. Found: C, 70.24; H, 6.72; N, 18.47.

Aufarbeitung

  1. filtrationthe resulting beige precipitate was filtered off
  2. washwashed with water
  3. customair-dried
  4. temperatureThe mixture was refluxed for 90 minutes
  5. customcollected the beige precipitate
  6. filtrationby filtration
  7. washrinsed with water
  8. customair-dried
  9. customdried to constant weight

Quellen und Nachweise

ORD-Eintrag
ord-a30618991393471a99e1b2d74406318a
Quelldatensatz
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07375126B2

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