Dichloromethane → HCID 13799792, Verbindung

HRID 1906395Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1906395
[CH3:1][C:2]([NH:6][S:7]([CH2:10][CH2:11][CH2:12][Cl:13])(=[O:9])=[O:8])([CH3:5])[C:3]#[N:4].[Cl:14][CH:15]([S:20]Cl)[C:16](Cl)([Cl:18])[Cl:17].[OH-].[Na+].C(Cl)[Cl:25]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.O>[Cl:25][C:15]([Cl:14])([S:20][N:6]([C:2]([C:3]#[N:4])([CH3:1])[CH3:5])[S:7]([CH2:10][CH2:11][CH2:12][Cl:13])(=[O:8])=[O:9])[CH:16]([Cl:18])[Cl:17]

Komponenten

7

Edukt 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 13799782HCID 13799782, Verbindung2×HCID 20211738Tetrachloroethylsulfenyl chloride

Produkt 1

HCID 13799792HCID 13799792, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 66133Benzyl triethylammonium chlorideKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred mixture of 2.25 g (0.01 mole) 2-methyl-2-(3-chloropropylsulfonamido)propionitrile (the product of Example 35) and 2.87 g (0.011 mole) tetrachloroethylsulfenyl chloride with 0.1 g benzyltriethylammonium chloride in 100 ml methylene chloride, 0.48 g [(0.012 mole) 0.96 g as a 50% weight/weight solution] sodium hydroxide dissolved in 20 ml water was added slowly. The reaction mixture was stirred for three hours. The mixture was washed three times with 100 ml water. The organic layers were dried over calcium sulfate and evaporated to give a dark brown oil which crystallized upon standing overnight. The crystals were washed with hexane to give the above-identified product, as a brown solid, melting point 68°-71° C.

Aufarbeitung

  1. additionwas added slowly
  2. washThe mixture was washed three times with 100 ml water
  3. dry with materialThe organic layers were dried over calcium sulfate
  4. customevaporated
  5. customto give a dark brown oil which
  6. customcrystallized
  7. waitupon standing overnight
  8. washThe crystals were washed with hexane
  9. customto give the above-identified product

Quellen und Nachweise

ORD-Eintrag
ord-2d4d96b7de5843a2be97d7e55488460c
Quelldatensatz
uspto-grants-1987_03
Patentnummer
US04652556

Notizen zur Reaktion

Wird geladen…