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HCID 58027707, Verbindung → HCID 20977333, Verbindung

HRID 716800
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 716800
[OH:1][CH:2]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([OH:12])[CH:7]=1)[CH2:3][C:4]#[N:5]>C1COCC1>[NH2:5][CH2:4][CH2:3][CH:2]([C:6]1[CH:7]=[C:8]([OH:12])[CH:9]=[CH:10][CH:11]=1)[OH:1]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 58027707HCID 58027707, Verbindung

Produkt 1

HCID 20977333HCID 20977333, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirred solution of the nitrile 21.16 (25.0 g, 153 mmol) in THF, cooled to 0° C., was added BH3-DMS (49.5 mL, 460 mmol), following which the cooling bath was removed. The resulting mixture was boiled under reflux overnight, cooled in an ice-bath and quenched by the slow addition of large excess of MeOH. After stirring at room temperature for 2 h, the excess solvent was removed under reduced pressure. The residue was again treated with MeOH and evaporated. The process was repeated three times. The brown oil was then applied onto a flash silica gel column and eluted (0 to 15% (9:1 MeOH—NH3)-DCM gradient) to give 3-(3-amino-1-hydroxypropyl)phenol (21.17) as a brown solid. Yield (25.0 g, 97%); 1H NMR (400 MHz, DMSO-d6) δ 7.04-7.09 (m, 1H), 6.74 (s, 1H), 6.70 (d, J=7.6 Hz, 1H), 6.58 (dd, J=8.0, 2.0 Hz, 1H), 4.55 (dd, J=7.2, 5.6 Hz, 1H), 2.57-2.66 (m, 2H), 1.56-1.62 (m, 2H).

Aufarbeitung

  1. customwas removed
  2. temperatureunder reflux overnight
  3. temperaturecooled in an ice-bath
  4. customquenched by the slow addition of large excess of MeOH
  5. customthe excess solvent was removed under reduced pressure
  6. additionThe residue was again treated with MeOH
  7. customevaporated
  8. washeluted (0 to 15% (9:1 MeOH—NH3)-DCM gradient)

Quellen und Nachweise

ORD-Eintrag
ord-cf9dd680c5e9435da679eac65211f346
Quelldatensatz
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09193669B2

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