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Potassium Iodide → HCID 86701104, Verbindung

HRID 1396245
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1396245
[CH3:1][O:2][C:3]1[CH:36]=[CH:35][C:6]([CH2:7][O:8][C@@H:9]2[C@@H:17](/[CH:18]=[CH:19]/[O:20]C)[O:16][C@H:15]3[C@H:11]([N:12]=[C:13]([N:22]([CH3:24])[CH3:23])[S:14]3)[C@H:10]2[O:25][CH2:26][C:27]2[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=2)=[CH:5][CH:4]=1.[I-].[K+]>C(#N)C.O.[Hg](OC(C)=O)OC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][O:8][C@@H:9]2[C@@H:17]([CH2:18][CH:19]=[O:20])[O:16][C@H:15]3[C@H:11]([N:12]=[C:13]([N:22]([CH3:24])[CH3:23])[S:14]3)[C@H:10]2[O:25][CH2:26][C:27]2[CH:28]=[CH:29][C:30]([O:33][CH3:34])=[CH:31][CH:32]=2)=[CH:35][CH:36]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 4875Potassium IodideHCID 69082734HCID 69082734, Verbindung

Produkt 1

HCID 86701104HCID 86701104, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 16683746DiacetyloxymercuryKatalysatorHCID 962WaterLösungsmittel2×
HCID 6342
Acetonitrile
Lösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a cold solution of 37 (100 mg, 0.18 mmol) in acetonitrile (20 mL) at −5° C. was added a solution of Hg(OAc)2 (68 mg, 0.21 mmol) in water (10 mL) dropwise. After stirred at 0° C. for 4 h, the reaction mixture was treated with potassium iodide (40 mg, 0.24 mmol) in water (1.6 mL) for 10 min. The reaction solution was quenched with water, extracted with dichloromethane (40 mL), and dried over MgSO4. Removal of solvents gave crude 2-((3aR,5R,6R,7R,7aR)-6,7-bis(4-methoxybenzyloxy)-2-(dimethylamino)-5,6,7,7a-tetrahydro-3aH-pyrano[3,2-d]thiazol-5-yl)acetaldehyde. To a solution of the crude product in dry THF (20 mL) was added NaBH4 (16 mg, 0.42 mmol) at 0° C. in portions. After stirred at 0° C. overnight, the reaction solution was quenched with water (25 mL) and extracted with ethyl acetate (2×20 mL). The combined organic phases were washed with saturated aqueous NH4Cl, dried over MgSO4, and concentrated to give a residue, which was purified by silica gel chromatography, eluted with 20-50% ethyl acetate in petroleum ether to give the product 38 as a light yellow oil (50 mg, 48%). (ES, m/z)[M+H]+ 503.0; 1H NMR (300 MHz, CDCl3) δ 7.15-7.35 (m, 4H), 6.84-6.98 (m, 4H), 6.28 (d, J=6.3 Hz, 1H), 4.45-4.89 (m, 4H), 4.18 (t, J=5.7 Hz, 1H), 3.94 (t, J=4.8 Hz, 1H), 3.87-3.91 (m, 1H), 3.78 (s, 6H), 3.56-3.65 (m, 3H), 2.92 (s, 6H), 1.89-1.98 (m, 1H), 1.62-1.73 (m, 1H).

Aufarbeitung

  1. customThe reaction solution was quenched with water
  2. extractionextracted with dichloromethane (40 mL)
  3. dry with materialdried over MgSO4
  4. customRemoval of solvents

Quellen und Nachweise

ORD-Eintrag
ord-42999f579a804fa287d6a22c29ac842a
Quelldatensatz
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08901087B2

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