1,2-Benzenedimethanol → N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine

HRID 258157

Reaktionsgleichung

Reaktionsgleichung von HRID 258157
[OH:1][CH2:2][C:3]1[C:4](=[CH:7][CH:8]=[CH:9][CH:10]=1)[CH2:5][OH:6].[CH:11]([N:14]([P:18](N(C(C)C)C(C)C)Cl)[CH:15]([CH3:17])[CH3:16])([CH3:13])[CH3:12]>C1COCC1>[CH:11]([N:14]([CH:15]([CH3:17])[CH3:16])[P:18]1[O:6][CH2:5][C:4]2[CH:7]=[CH:8][CH:9]=[CH:10][C:3]=2[CH2:2][O:1]1)([CH3:13])[CH3:12]

Komponenten

4

Edukt 2

HCID 691531,2-Benzenedimethanol2×HCID 2733425Bis(diisopropylamino)chlorophosphine

Produkt 1

HCID 19782585N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Phthalyl alcohol (1.15 g, 8.31 mmol) was dissolved in 5 ml of THF, and bisdiisopropylaminochlorophosphine (2.21 g, 8.31 mmol) which was dissolved in 5 ml of THF was added dropwise to the solution at -15° C. under a nitrogen atmosphere. Afterward, the temperature of the solution was adjusted to room temperature, and after the disappearance of phthalyl alcohol had been confirmed, hydrochloride of diisopropylamine was washed with ether. The wash liquor was concentrated and then distilled in order to obtain the desired product having a melting point of from 150° to 155° C. (0.7 mmHg).

Aufarbeitung

  1. additionwas added dropwise to the solution at -15° C. under a nitrogen atmosphere
  2. customwas adjusted to room temperature
  3. washhydrochloride of diisopropylamine was washed with ether
  4. concentrationThe wash liquor was concentrated
  5. distillationdistilled in order

Quellen und Nachweise

ORD-Eintrag
ord-9d568a1daaed4c6d917cab90fc95f644
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05264605

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