Chloroform → HCID 20084584, Verbindung

HRID 1609283Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1609283
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][C:17](=[O:32])[C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29](=[O:31])[CH3:30])=[CH:20][CH:19]=1)#[N:2].[BH4-].[Na+].C(Cl)(Cl)Cl>O1CCCC1.CO>[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][C:17](=[O:32])[C:18]1[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH:29]([OH:31])[CH3:30])=[CH:22][CH:23]=1)#[N:2]

Komponenten

6

Edukt 3

HCID 6212ChloroformHCID 4311764Sodium borohydrideHCID 20084436HCID 20084436, Verbindung

Produkt 1

HCID 20084584HCID 20084584, VerbindungAusbeute 94,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In 30 ml of tetrahydrofuran was suspended 3.33 g of N-[2-(2-cyanophenylthio)phenyl]-4-(5-oxohexyloxy)benz-amide (prepared in accordance with Reference Example 6, Step 2) followed by addition of a solution of 0.31 g of sodium borohydride in methanol, and the mixture was stirred for 1 hour. To the reaction mixture was added chloroform and the mixture was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethyl acetate-n-hexane to give 3.15 g of the title compound as white crystals.

Aufarbeitung

  1. washthe mixture was washed with saturated aqueous sodium chloride solution
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was recrystallized from ethyl acetate-n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-e5124195e9134832b1331333fe0b7e28
Quelldatensatz
uspto-grants-1995_03
Patentnummer
US05399703

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