tert-Butyl methyl ether → Didodecyl 2-(t-butylthio)-1-hydroxy-1-methylethanephosphonate

HRID 1079098Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1079098
[P:1]([O-:28])([O:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].COC(C)(C)C.N12CCCNC1C=CCCC2.[C:46]([S:50][CH2:51][C:52](=[O:54])[CH3:53])([CH3:49])([CH3:48])[CH3:47]>C1(C)C=CC=CC=1.CS(C)=O>[C:46]([S:50][CH2:51][C:52]([OH:54])([CH3:53])[P:1]([O:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])(=[O:28])[O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])([CH3:49])([CH3:48])[CH3:47]

Komponenten

7

Edukt 4

HCID 15413tert-Butyl methyl etherHCID 114236691-(Tert-butylsulfanyl)propan-2-oneHCID 150726561,2,3,4,6,7,8,10A-octahydropyrimido[1,2-a]azepineHCID 21884946CID 21884946

Produkt 1

HCID 19428699Didodecyl 2-(t-butylthio)-1-hydroxy-1-methylethanephosphonate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

23.0 g (55 mmol) of didodecyl phosphite are initially introduced into a mixture of 20 ml of tert-butyl methyl ether and 5 ml of dimethyl sulfoxide. 1.0 g of 1,8-diazabicyclo[5.4.0]undec-5-ene (DBU) are added, and 8.04 g (55 mmol) of (t-butylthio)acetone are then added dropwise at 30° C. The reaction mixture is heated for 5 hours at 60° C., cooled, diluted with 150 ml of toluene and washed with 100 ml of water. The organic phase is dried over sodium sulfate, and the solvent and remainders of the educts are distilled off in vacuo (finally at 0.5 mbar and 55° C. bath temperature).

Aufarbeitung

  1. temperaturecooled
  2. washwashed with 100 ml of water
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. distillationthe solvent and remainders of the educts are distilled off in vacuo (finally at 0.5 mbar and 55° C. bath temperature)

Quellen und Nachweise

ORD-Eintrag
ord-b5843fedb2dc44da9fcd9d43da58a25d
Quelldatensatz
uspto-grants-1996_08
Patentnummer
US05550276

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