Benzene → 2,2-Dichloro-1-(1-oxa-5-azaspiro[5.5]undecan-5-yl)ethan-1-one

HRID 127485Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 127485
[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[NH2:8][CH2:9][CH2:10][CH2:11]O.C1C=CC=CC=1.[Cl:19][CH:20]([Cl:24])[C:21](Cl)=[O:22]>O>[Cl:19][CH:20]([Cl:24])[C:21]([N:8]1[C:1]2([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[O:7][CH2:11][CH2:10][CH2:9]1)=[O:22]

Komponenten

6

Edukt 4

HCID 241BenzeneHCID 6593Dichloroacetyl chlorideHCID 7967CyclohexanoneHCID 90863-Amino-1-propanol

Produkt 1

HCID 132772052,2-Dichloro-1-(1-oxa-5-azaspiro[5.5]undecan-5-yl)ethan-1-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

From a boiling mixture of 17.6 g. (0.18 moles) of cyclohexanone and 11.2 g. (0.15 moles) of 3-aminopropanol in 50 ml. of benzene the water formed is continuously distilled off. Boiling is continued until 2.7 ml. of water are separated. The reaction mixture is then cooled and 16 ml. (0.165 moles) of a 40% aqueous sodium hydroxide solution are added followed by a subsequent dropwise addition of 22.1 g. (0.15 moles) of dichloroacetyl chloride, with external salt/ice cooling.

Aufarbeitung

  1. additionFrom a boiling mixture of 17.6 g
  2. distillationis continuously distilled off
  3. customof water are separated
  4. temperatureThe reaction mixture is then cooled
  5. addition(0.165 moles) of a 40% aqueous sodium hydroxide solution are added
  6. additionfollowed by a subsequent dropwise addition of 22.1 g

Quellen und Nachweise

ORD-Eintrag
ord-d40a2305369442aa974c6de9b8e13141
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04256481

Notizen zur Reaktion

Wird geladen…