Sodium borohydride → Tricyclohexylstannane

HRID 501919

Reaktionsgleichung

Reaktionsgleichung von HRID 501919
C(OCC)C.O.[BH4-].[Na+].[OH-].[CH:10]1([Sn+:16]([CH:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)[CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1>C(OCC)C>[CH:23]1([SnH:16]([CH:10]2[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]2)[CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1

Komponenten

5

Edukt 3

HCID 4311764Sodium borohydrideHCID 9864905CyhexatinHCID 21584184Diethylether water

Produkt 1

HCID 25729Tricyclohexylstannane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture (400 mL) of diethyl oxide:water 1:1 was cooled at 0° C. under nitrogen in a three-necked flask of 1 L. Sodium borohydride (3 g, 79.4 mmol) and then tricyclohexyltin hydroxide (30 g, 62.2 mmol) were successively and carefully added. After addition of 100 mL of diethyl oxide, the mixture was stirred 2 days at room temperature. After separation, the organic layer was dried over magnesium sulphate and evaporated under reduced pressure. The crude product was distilled under high vacuum to afford, a colourless oil (23.23 g; 63 mmol).

Aufarbeitung

  1. additioncarefully added
  2. customAfter separation
  3. dry with materialthe organic layer was dried over magnesium sulphate
  4. customevaporated under reduced pressure
  5. distillationThe crude product was distilled under high vacuum
  6. customto afford

Quellen und Nachweise

ORD-Eintrag
ord-e9984706c97648daa4d4da5956ff6f64
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772417B2

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