Trichloroacetic Acid → 2-[2-(bis-(2-chloroethyl)-amino)-6-methyl-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid cyclohexylammonium salt

HRID 1651522Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1651522
[Cl:1][CH2:2][CH2:3][N:4]([CH2:14][CH2:15][Cl:16])[P:5]1(=[O:13])[NH:10][CH:9](O)[CH2:8][CH:7]([CH3:12])[O:6]1.[CH:17]1([NH3+:23])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.[SH:24][CH2:25][CH2:26][S:27]([O-:30])(=[O:29])=[O:28].ClC(Cl)(Cl)C(O)=O>O.CC(C)=O>[CH:17]1([NH3+:23])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.[Cl:1][CH2:2][CH2:3][N:4]([CH2:14][CH2:15][Cl:16])[P:5]1(=[O:13])[NH:10][CH:9]([S:24][CH2:25][CH2:26][S:27]([O-:30])(=[O:29])=[O:28])[CH2:8][CH:7]([CH3:12])[O:6]1

Komponenten

6

Edukt 3

HCID 6421Trichloroacetic AcidHCID 230498732-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1)HCID 230498752-(bis-(2-chloroethyl)-amino)-4-hydroxy-6-methyl-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide

Produkt 1

HCID 1317149752-[2-(bis-(2-chloroethyl)-amino)-6-methyl-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid cyclohexylammonium salt

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

1.45 g (5 mmol) of 2-(bis-(2-chloroethyl)-amino)-4-hydroxy-6-methyl-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide and 1.2 g (5 mmol) of cyclohexylammonium-2-mercaptoethanesulphonate were dissolved in 5 ml of water and in 5 ml of acetone, acidified with trichloroacetic acid and left to stand for 20 hours at 0° C. The mixture was then filtered, the filtrate was carefully concentrated under vacuum, the residue was taken up twice in acetone and was concentrated. The residue was then dissolved in acetone, precipitated with ether, washed with ether and dried.

Aufarbeitung

  1. waitleft
  2. filtrationThe mixture was then filtered
  3. concentrationthe filtrate was carefully concentrated under vacuum
  4. concentrationwas concentrated
  5. dissolutionThe residue was then dissolved in acetone
  6. customprecipitated with ether
  7. washwashed with ether
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9ae26238ee444e2a9a96fff4b1bfdf3a
Quelldatensatz
uspto-grants-1990_05
Patentnummer
US04929607

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