Pilocarpine → Pilocarpine Alpha Tocopherol Hemisuccinate

HRID 1723310

Reaktionsgleichung

Reaktionsgleichung von HRID 1723310
[CH3:1][CH2:2][C@@H:3]1[C:7](=[O:8])[O:6][CH2:5][C@@H:4]1[CH2:9][C:10]1[N:14]([CH3:15])[CH:13]=[N:12][CH:11]=1.[CH3:16][C:17]1[C:22]([CH3:23])=[C:21]([O:24][C:25]([CH2:27][CH2:28][C:29]([OH:31])=[O:30])=[O:26])[C:20]([CH3:32])=[C:19]2[CH2:33][CH2:34][C@:35]([CH2:38][CH2:39][CH2:40][C@@H:41]([CH2:43][CH2:44][CH2:45][C@@H:46]([CH2:48][CH2:49][CH2:50][CH:51]([CH3:53])[CH3:52])[CH3:47])[CH3:42])([CH3:37])[O:36][C:18]=12.CC1C(C)=C2C(CC[C@](CCC[C@@H](CCC[C@@H](CCCC(C)C)C)C)(C)O2)=C(C)C=1O>C(Cl)Cl>[CH3:1][CH2:2][C@@H:3]1[C:7](=[O:8])[O:6][CH2:5][C@@H:4]1[CH2:9][C:10]1[N:14]([CH3:15])[CH:13]=[N:12][CH:11]=1.[CH3:16][C:17]1[C:22]([CH3:23])=[C:21]([O:24][C:25]([CH2:27][CH2:28][C:29]([OH:31])=[O:30])=[O:26])[C:20]([CH3:32])=[C:19]2[CH2:33][CH2:34][C@:35]([CH2:38][CH2:39][CH2:40][C@@H:41]([CH2:43][CH2:44][CH2:45][C@@H:46]([CH2:48][CH2:49][CH2:50][CH:51]([CH3:53])[CH3:52])[CH3:47])[CH3:42])([CH3:37])[O:36][C:18]=12

Komponenten

5

Edukt 3

HCID 5910Pilocarpine2×HCID 14985alpha-TocopherolHCID 20353alpha-Tocopherol succinate

Produkt 1

HCID 131716046Pilocarpine Alpha Tocopherol Hemisuccinate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

Five grams of pilocarpine base were added to a weighed 500 ml round bottom flask and stopper, and the total mass in grams recorded. D-alpha-tocopherol acid succinate (12.75 g, corresponding to a 1:1M ratio of pilocarpine:D-alpha-tocopherol) was added to the flask and the contents again weighed. Methylene chloride (50 ml) was added and the flask agitated to dissolve the solids and the flask again weighed. The flask was placed on a rotary evaporator in a water bath at 55° C. and rotated for 30 minutes (no vacuum applied). After 30 minutes, the flask and contents were again weighed, then rotary evaporated with vacuum at 55° C. The weight of the flask was recorded every 30 minutes thereafter until two successive weighings were within 0.1 g. The preparation was then cooled to room temperature (25° C.), stoppered, and stored at 4° C.

Aufarbeitung

  1. dissolutionto dissolve the solids
  2. customThe flask was placed on a rotary evaporator in a water bath at 55° C.
  3. waitAfter 30 minutes
  4. customrotary evaporated with vacuum at 55° C
  5. waitThe weight of the flask was recorded every 30 minutes
  6. customstored at 4° C.

Quellen und Nachweise

ORD-Eintrag
ord-b4f7990c8dc145e58418d4781472d9ef
Quelldatensatz
uspto-grants-1989_08
Patentnummer
US04861580

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