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Trifluoroacetic acid → HCID 71554976, Verbindung

HRID 2281672
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2281672
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[C:14]3([CH2:17][N:16]([C:18](OC(C)(C)C)=[O:19])[CH2:15]3)[CH2:13][CH2:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.[Cl:32][C:33]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]=1[CH2:40][N:41]=C=O.C(N(CC)CC)C>ClCCl.C(#N)C>[Cl:32][C:33]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]=1[CH2:40][NH:41][C:18]([N:16]1[CH2:15][C:14]2([N:11]([S:8]([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)(=[O:9])=[O:10])[CH2:12][CH2:13]2)[CH2:17]1)=[O:19]
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Komponenten

7

Edukt 4

HCID 6422Trifluoroacetic acid2×HCID 8471TriethylamineHCID 46127082,4-Dichlorobenzyl isocyanateHCID 86682348HCID 86682348, Verbindung

Produkt 1

HCID 71554976HCID 71554976, VerbindungAusbeute 91,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342
Acetonitrile
Lösungsmittel
HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of tert-butyl 1-(4-fluorophenylsulfonyl)-1,6-diazaspiro[3.3]heptane-6-carboxylate (452 mg, 1.27 mmol) in dichloromethane (8 mL) was added trifluoroacetic acid (489 μl, 6.34 mmol). After 2 h at ambient temperature, another amount of trifluoroacetic acid was added (300 μl, 3.89 mmol). The reaction mixture was stirred for 1.5 h at ambient temperature and concentrated under reduced pressure. The residue was partitioned in toluene (10 mL) and then concentrated, this procedure was repeated twice to give the unpurified amine (540 mg), which was used directly in the next step without further purification. To a solution of the obtained 1-(4-fluorophenylsulfonyl)-1,6-diazaspiro[3.3]heptanes in acetonitrile (10 mL) was added 2,4-dichloro-1-(isocyanatomethyl)benzene (216 μl, 1.47 mmol) followed by triethylamine (294 μl, 2.11 mmol) and the mixture was stirred for 1 h at ambient temperature. The solvent was evaporated in vacuo and the resulting solid was purified by chromatography (SiO2; heptane:ethyl acetate 1:4 to dichloromethane/methanol/ammonia 95:4.5:0.5) to give the titled compound (530 mg, 91%) as colorless solid. HRMS (EI): 457.0431 (exact mass calculated for C19H17Cl2FN3O3S ([M]+)=457.0430).

Aufarbeitung

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was partitioned in toluene (10 mL)
  3. concentrationconcentrated
  4. customto give the unpurified amine (540 mg), which
  5. customwas used directly in the next step without further purification
  6. stirringthe mixture was stirred for 1 h at ambient temperature
  7. customThe solvent was evaporated in vacuo
  8. customthe resulting solid was purified by chromatography (SiO2; heptane:ethyl acetate 1:4 to dichloromethane/methanol/ammonia 95:4.5:0.5)

Quellen und Nachweise

ORD-Eintrag
ord-d2261def993a4c32bb6bf5fda3f9e2fa
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09139593B2

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