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Formaldehyde → tert-butyl (6S,7S)-5-methyl-6-{[4-(3-methylphenyl)piperazin-1-yl]carbonyl}-5-azaspiro[2.5]octane-7-carboxylate

HRID 1664606
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1664606
[C:1]([O:5][C:6]([C@H:8]1[CH2:15][C:12]2([CH2:14][CH2:13]2)[CH2:11][NH:10][C@@H:9]1[C:16]([OH:18])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=C[C:29]=2N=N1.[CH3:46][C:47]1[CH:48]=[C:49]([N:53]2[CH2:58][CH2:57][NH:56][CH2:55][CH2:54]2)[CH:50]=[CH:51][CH:52]=1.C(N(C(C)C)CC)(C)C.C=O.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>CN(C=O)C>[CH3:29][N:10]1[C@H:9]([C:16]([N:56]2[CH2:57][CH2:58][N:53]([C:49]3[CH:50]=[CH:51][CH:52]=[C:47]([CH3:46])[CH:48]=3)[CH2:54][CH2:55]2)=[O:18])[C@@H:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:15][C:12]2([CH2:13][CH2:14]2)[CH2:11]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 712FormaldehydeHCID 81531DiisopropylethylamineHCID 831111-(m-Tolyl)piperazineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 5049666Sodium triacetoxyborohydrideHCID 16108946HCID 16108946, Verbindung

Produkt 1

HCID 67438575tert-butyl (6S,7S)-5-methyl-6-{[4-(3-methylphenyl)piperazin-1-yl]carbonyl}-5-azaspiro[2.5]octane-7-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of (6S,7S)-7-(tert-butoxycarbonyl)-5-azaspiro[2.5]octane-6-carboxylic acid of step 1g (25 mg), BOP (45 mg), 1-(3-methylphenyl)piperazine (176 mg) and di-isopropylethylamine (70 μL) in DMF (500 μL) was stirred at RT overnight. Formaldehyde solution (0.5 M in THF/MeCN (1:1), 600 μL) was added to the mixture followed by NaBH(OAc)3 (0.25 M in THF/MeCN (1:1), 1000 μL). The resulting mixture was stirred overnight. The solvents were removed under reduced pressure. The residue was dissolved in ethyl acetate (5 mL). The solution was washed with NaHCO3 (7.5%, 3×1 mL). The organic phase was dried over MgSO4 and filtered and concentrated. The residue was used directly in the next step reaction without further purification.

Aufarbeitung

  1. stirringThe resulting mixture was stirred overnight
  2. customThe solvents were removed under reduced pressure
  3. dissolutionThe residue was dissolved in ethyl acetate (5 mL)
  4. washThe solution was washed with NaHCO3 (7.5%, 3×1 mL)
  5. dry with materialThe organic phase was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was used directly in the next step reaction without further purification

Quellen und Nachweise

ORD-Eintrag
ord-64cd5d86318a4007becad14845274bf5
Quelldatensatz
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08039471B2

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