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Benzylamine → HCID 20679455, Verbindung

HRID 651344
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 651344
ON1C2C=CC=CC=2N=N1.C(N=C=NC(C)C)(C)C.C(N(CC)C(C)C)(C)C.[CH2:29]([NH2:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[C:51]1([CH2:61][N:62]2[CH2:82][CH2:81][C:65]3([N:69]([C:70]4[CH:75]=[CH:74][CH:73]=[CH:72][CH:71]=4)[CH2:68][N:67]([CH2:76][C:77](O)=[O:78])[C:66]3=[O:80])[CH2:64][CH2:63]2)[C:60]2[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=2)[CH:54]=[CH:53][CH:52]=1>CN(C)C=O.ClCCCl>[CH2:29]([NH:36][C:77](=[O:78])[CH2:76][N:67]1[C:66](=[O:80])[C:65]2([CH2:81][CH2:82][N:62]([CH2:61][C:51]3[C:60]4[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=4)[CH:54]=[CH:53][CH:52]=3)[CH2:63][CH2:64]2)[N:69]([C:70]2[CH:75]=[CH:74][CH:73]=[CH:72][CH:71]=2)[CH2:68]1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 7504BenzylamineHCID 12734Diisopropylcarbodiimide2×HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 9932381HCID 9932381, Verbindung

Produkt 1

HCID 20679455
HCID 20679455, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 111,2-DichloroethaneLösungsmittelHCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

To a suspension of the the commercially available aminomethylated polystyrene resin (Novabiochem) (20 g, 16 mmol) in dimethylformamide (70 ml) was added a solution of the commercially available BAL-Linker (PerSeptive Biosystems GMBH) (12.88 g, 48.0 mmol) and 1-hydroxybenzotriazole (7.26 g, 48.0 mmol) in 70 ml of dimethylformamide. To this was added N,N′-diisopropylcarbodiimide (6.06 g, 48.0 mmol) followed by N,N-diisopropylethylamine (6.19 g, 48.0 mmol). The reaction was allowed to stir 20 h at room temperature. The resin was filtered and washed as follows: 3×dimethylformamide (50 ml), 3×tetrahydrofuran (50 ml), 3×dichloromethane (50 ml), 3×ether (50 ml). The resin was dried in vacuo and isolated: 23.92 g. IR spectroscopy showed an aldehyde stretching band at 1674 cm−1. To a part of this resin (0.200 g, 0.160 mmol) in 1,2-dichloroethane (8 ml) at room temperature, was added benzyl amine (0.171 g, 1.60 mmol) followed by sodium triacetoxyborohydride (0.339 g, 1.60 mmol). The reaction was allowed to shake 20 h at room temperature, filtered and washed as follows: 3×dimethylformamide/water (90/10) (8 ml); 3×dimethylformamide (8 ml); 3×dichloromethane (8 ml). The resin was suspended in dimethylformamide, treated with (8-naphthalen-1-ylmethyl-4-oxo-1-phenyl-1,3,8-triaza-spiro[4.5]dec-3-yl)-acetic acid (0.274 g, 0.640 mmol), 1-hydroxybenzotrazole (0.099 9, 0.640 mmol) and N,N′-diisopropylcarbodiimide (0.081 g, 0.640 mmol). The reaction was allowed to shake for 20 h at room temperature. The resin was filtered, suspended in dimethylsulfoxide and heated to 40° C. for 1 h. The resin was again filtered, suspended in dimethylsulfoxide (8 ml) and heated to 40° C. for 1 h. The resin was filtered and washed as follows: 3×dimethylformamide/water (90/10) (8 ml); 3×dimethylformamide (8 ml); 3×dichloromethane (8 ml) and air-dried. The resin was treated with trifluoroacetic acid/water (95/5) (8 ml) for 1 h at room temperature. The filtrate was collected and concentrated in vacuo to give the desired product.

Aufarbeitung

  1. filtrationThe resin was filtered
  2. washwashed
  3. customThe resin was dried in vacuo
  4. customisolated
  5. waitto shake 20 h at room temperature
  6. filtrationfiltered
  7. washwashed
  8. waitto shake for 20 h at room temperature
  9. filtrationThe resin was filtered
  10. temperatureheated to 40° C. for 1 h
  11. filtrationThe resin was again filtered
  12. temperatureheated to 40° C. for 1 h
  13. filtrationThe resin was filtered
  14. washwashed
  15. dry with material3×dichloromethane (8 ml) and air-dried
  16. additionThe resin was treated with trifluoroacetic acid/water (95/5) (8 ml) for 1 h at room temperature
  17. customThe filtrate was collected
  18. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-78fa766f8a7c46358e21af3d2a5f59a0
Quelldatensatz
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06277991B1

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