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Hydrochloric Acid → 2-[1,3,6,2]Dioxazaborocan-2-yl-4-trifluoromethyl-benzoic acid 2,2-dimethyl-propyl ester

HRID 1870568
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1870568
[CH3:1][C:2]([CH3:18])([CH3:17])[CH2:3][O:4][C:5](=[O:16])[C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][CH:7]=1.[CH:19]([O:22][B:23](OC(C)C)[O:24][CH:25]([CH3:27])C)(C)[CH3:20].C([N-:35]C(C)C)(C)C.[Li+].Cl.N(CCO)CCO>O1CCCC1.O1CCCC1.CCCCCCC.C(O)(C)C>[CH3:1][C:2]([CH3:18])([CH3:17])[CH2:3][O:4][C:5](=[O:16])[C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:13])([F:14])[F:15])=[CH:8][C:7]=1[B:23]1[O:24][CH2:25][CH2:27][NH:35][CH2:20][CH2:19][O:22]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 8113DiethanolamineHCID 21531Triisopropyl borateHCID 599219Neopentyl 4-(trifluoromethyl)benzoateHCID 2724682Lithium diisopropylamide

Produkt 1

HCID 107143722-[1,3,6,2]Dioxazaborocan-2-yl-4-trifluoromethyl-benzoic acid 2,2-dimethyl-propyl ester
Ausbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 3776IsopropanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 21263495Tetrahydrofuran heptaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of 4-trifluoromethyl-benzoic acid 2,2-dimethyl-propyl ester (35.8 g, 138 mmol) in tetrahydrofuran (250 mL) was added triisopropylborate (73.0 mL, 316 mmol). The solution was cooled to 0° C., lithium diisopropylamide (73.0 mL of a 2.0M solution in tetrahydrofuran/heptane, 146.0 mmol) was added dropwise over 20 minutes, and the red solution was stirred for an additional 30 minutes. Hexanes (200 mL) was added followed by 1N hydrochloric acid (200 mL). The mixture was stirred for 10 minutes and poured into hexanes (200 mL). The organic layer was washed with 1N hydrochloric acid (two times 150 mL), and brine (100 mL). The organic extracts were dried over magnesium sulfate, filtered, and concentrated to about 200 mL. Isopropyl alcohol (100 mL), and diethanolamine (15.95 g, 151.7 mmol) were added, and the mixture was stirred at room temperature for 10 hours. The solids were filtered and washed with a mixture of isopropyl alcohol (15 mL) and hexanes (30 mL) to provide 2-[1,3,6,2]dioxazaborocan-2-yl-4-trifluoromethyl-benzoic acid 2,2-dimethyl-propyl ester (37.83 g, 74% yield) as a white solid. mp=233-234° C; IR 3077, 2963, 2862, 1722, 1480, 1467, 1371, 1331, 1298, 1290, 1279, 1254, 1161, 1117, 1108, 1087, 1074, 995, 952, 862, cm-1, 1H NMR (400 MHz, CDCl3) δ 8.23 (s, 1H), 7.72 (d, J=7.9 Hz, 1H), 7.52 (dd, J=7.9, 1.3 Hz, 1H), 6.33 (brs, 1H), 4.08-4.14 (m, 2H), 3.98 (s, 2H), 3.93-3.98 (m, 2H), 3.42-3.50 (m, 2H), 2.88-2.94 (m, 2H), 1.02 (s, 9H); 13C NMR (100 MHz, CDCl3) 26.51, 31.69, 50.92, 63.33, 74.72, 123.94, 128.59, 132.06, 139.61, 171.56.

Aufarbeitung

  1. stirringThe mixture was stirred for 10 minutes
  2. washThe organic layer was washed with 1N hydrochloric acid (two times 150 mL), and brine (100 mL)
  3. dry with materialThe organic extracts were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to about 200 mL
  6. stirringthe mixture was stirred at room temperature for 10 hours
  7. filtrationThe solids were filtered
  8. washwashed with a mixture of isopropyl alcohol (15 mL) and hexanes (30 mL)

Quellen und Nachweise

ORD-Eintrag
ord-2b6332b282bf43deb4a5cb991df82d2d
Quelldatensatz
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06096906

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