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Dichloromethane → (2R)-2-({4-[(2,1,3-Benzothiadiazol-5-ylmethyl)amino]-1-piperidinyl}methyl)-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione hydrochloride

HRID 1943209
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1943209
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]2[N:19]3[C:20]4[N:11]([C:12](=[O:22])[CH:13]=[CH:14][C:15]=4[N:16]=[CH:17][C:18]3=[O:21])[CH2:10]2)[CH2:4][CH2:3]1.[N:23]1[S:24][N:25]=[C:26]2[CH:31]=[C:30]([CH:32]=O)[CH:29]=[CH:28][C:27]=12.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+].[Cl:53]CCl>CO.C(Cl)(Cl)Cl>[ClH:53].[N:23]1[S:24][N:25]=[C:26]2[CH:31]=[C:30]([CH2:32][NH:1][CH:2]3[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]4[N:19]5[C:20]6[N:11]([C:12](=[O:22])[CH:13]=[CH:14][C:15]=6[N:16]=[CH:17][C:18]5=[O:21])[CH2:10]4)[CH2:4][CH2:3]3)[CH:29]=[CH:28][C:27]=12
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 6344DichloromethaneHCID 516892Sodium BicarbonateHCID 27762902,1,3-Benzothiadiazole-5-carbaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 58200877(2R)-2-[(4-Amino-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione

Produkt 1

HCID 68598539
(2R)-2-({4-[(2,1,3-Benzothiadiazol-5-ylmethyl)amino]-1-piperidinyl}methyl)-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

(2R)-2-[(4-Amino-1-piperidinyl)methyl]-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylene-3,8-dione (50 mg, 0.166 mmol) (for a preparation see Example 16(j)) and 2,1,3-benzothiadiazole-5-carbaldehyde (25 mg, 0.918 eq.) were stirred in 9:1 v:v chloroform:methanol (1 ml) for 2.5 hours. Sodium triacetoxyborohydride (105 mg, 3.000 eq.) was then added in one portion and the mixture was stirred vigorously at room temperature for 30 min. Saturated aqueous sodium hydrogen carbonate (0.5 ml) was then added, followed by dichloromethane (10 ml) and the mixture was stirred vigorously at room temperature for 10 min and the phases were separated (hydrophobic frit). The organic phase was evaporated under reduced pressure and the crude product was purified by column chromatography on silica (eluted with 0-12% (2M NH3 in MeOH) in DCM). Appropriate fractions were combined and evaporated under reduced pressure to give the free base of the title compound as a yellow solid (41 mg).

Aufarbeitung

  1. stirringthe mixture was stirred vigorously at room temperature for 30 min
  2. stirringthe mixture was stirred vigorously at room temperature for 10 min
  3. customthe phases were separated (hydrophobic frit)
  4. customThe organic phase was evaporated under reduced pressure
  5. customthe crude product was purified by column chromatography on silica (eluted with 0-12% (2M NH3 in MeOH) in DCM)
  6. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-80abed54041e471a9f8f3ea9f38c1384
Quelldatensatz
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08389524B2

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