Hydrochloric Acid → 3-Chloro-3-methyl-2-nitroso-1-butyl acetate

HRID 1076971

Reaktionsgleichung

Reaktionsgleichung von HRID 1076971
[C:1]([O:4][CH2:5][CH:6]=[C:7]([CH3:9])[CH3:8])(=[O:3])[CH3:2].[N:10]([O:12]CCC(C)C)=O.[ClH:18]>C(O)(=O)C>[C:1]([O:4][CH2:5][CH:6]([N:10]=[O:12])[C:7]([Cl:18])([CH3:9])[CH3:8])(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 14489Prenyl acetate

Produkt 1

HCID 540488323-Chloro-3-methyl-2-nitroso-1-butyl acetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Versuchsvorschrift

3,3-Dimethylallyl acetate (25 ml.), iso-amyl nitrite (45 ml.) and glacial acetic acid (65 ml.) were cooled in an ice-salt mixture. An ice-cold mixture of concentrated hydrochloric acid (20 ml.) and glacial acetic acid (20 ml.) was added gradually with stirring. The solution became green and towards the end of the addition a white solid precipitated. The solid was collected by filtration and dried (13 g.) Recrystallisation from CCl4 -- 40°/60° petrol gave the title compound as colourless needles (10 g.) m.p. 117°-119°.

Aufarbeitung

  1. additionwas added gradually
  2. additionThe solution became green and towards the end of the addition a white solid
  3. customprecipitated
  4. filtrationThe solid was collected by filtration
  5. customdried
  6. custom(13 g.) Recrystallisation from CCl4

Quellen und Nachweise

ORD-Eintrag
ord-61fa8655952e497390421b283761e33b
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03959278

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