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tert-Butanol → 4-[9-(N-t-butyloxycarbonylaminosulfonylamino)nonyl]-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman

HRID 1792311
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1792311
Cl[S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3].[C:8]([OH:12])([CH3:11])([CH3:10])[CH3:9].[NH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH:23]1[C:32]2[C:27](=[CH:28][C:29]([O:33][CH2:34][O:35][CH3:36])=[CH:30][CH:31]=2)[O:26][CH2:25][C:24]1([C:38]1[CH:43]=[CH:42][C:41]([O:44][CH2:45][O:46][CH3:47])=[CH:40][CH:39]=1)[CH3:37].C(N(CC)CC)C.[Cl-].[NH4+]>ClCCl>[C:8]([O:12][C:6]([NH:5][S:2]([NH:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH:23]1[C:32]2[C:27](=[CH:28][C:29]([O:33][CH2:34][O:35][CH3:36])=[CH:30][CH:31]=2)[O:26][CH2:25][C:24]1([C:38]1[CH:39]=[CH:40][C:41]([O:44][CH2:45][O:46][CH3:47])=[CH:42][CH:43]=1)[CH3:37])(=[O:4])=[O:3])=[O:7])([CH3:11])([CH3:10])[CH3:9]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 70918Chlorosulfonyl isocyanateHCID 220332874-(9-Aminononyl)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman

Produkt 1

HCID 22033418
4-[9-(N-t-butyloxycarbonylaminosulfonylamino)nonyl]-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman
Ausbeute 36 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

To a solution of chlorosulfonylisocyanate (25 μl, 0.292 mmol) in dichloromethane (1 ml) was added t-butanol (27 μl, 0.292 mmol) at −38° C. for 10 minutes, which was then stirred for 2.5 hours. Then, the reaction mixture was cooled down to −78° C., 4-(9-aminononyl)-7-methoxymethoxy-3-(4-methoxymethoxyphenyl)-3-methylchroman (118 mg, 0.243 mmol) dissolved in triethylamine (50 μl, 0.364 mmol) and dichloromethane (1 ml) was slowly added thereto, and the resulting mixture was stirred overnight at room temperature. After the reaction was completed, saturated ammonium chloride solution was added to the reaction solution, and the resulting solution was extracted with ethyl acetate. The organic layer was washed with diluted hydrochloride solution, water and saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The residue was subjected to preparative TLC (chloroform:methanol=10:1) to give the title compound (57 mg, yield 36%) as a white solid.

Aufarbeitung

  1. stirringthe resulting mixture was stirred overnight at room temperature
  2. extractionthe resulting solution was extracted with ethyl acetate
  3. washThe organic layer was washed with diluted hydrochloride solution, water and saturated sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-e1303aa57d08490ab4c08a11e97e8579
Quelldatensatz
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07074819B2

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