Rocuronium Bromide Impurity 31 → HCID 18637387, Verbindung

HRID 329957

Reaktionsgleichung

Reaktionsgleichung von HRID 329957
[C:1]([O:4][C@@H:5]1[C@@H:22]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[CH2:21][C@@:20]2([CH3:29])[C@@H:7]([CH2:8][CH2:9][C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[CH2:12][C@H:13]([N:34]3[CH2:38][CH2:37][CH2:36][CH2:35]3)[C@@H:14]2[O:30]C(=O)C)[CH2:6]1)(=[O:3])[CH3:2]>CO>[C:1]([O:4][C@@H:5]1[C@@H:22]([N:23]2[CH2:24][CH2:25][O:26][CH2:27][CH2:28]2)[CH2:21][C@@:20]2([CH3:29])[C@@H:7]([CH2:8][CH2:9][C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[CH2:12][C@H:13]([N:34]3[CH2:35][CH2:36][CH2:37][CH2:38]3)[C@@H:14]2[OH:30])[CH2:6]1)(=[O:3])[CH3:2]

Komponenten

3

Edukt 1

HCID 54054638Rocuronium Bromide Impurity 31

Produkt 1

HCID 18637387HCID 18637387, VerbindungAusbeute 85,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol diacetate (6.0 g) in methanol (70 ml) was set aside at room temperature for 20 h., during which time the product partially crystallised. Water (150 ml) was added to precipitate the product as a yellow solid, which was filtered off and dried. The crude solid was recrystallised from ethanol (110 ml) to give (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol 3-acetate (4.70 g), m.p. 112°-118° C.; [α]D20 =+33.1° (c 0.97 in CHCl3)

Aufarbeitung

  1. customthe product partially crystallised
  2. additionWater (150 ml) was added
  3. customto precipitate the product as a yellow solid, which
  4. filtrationwas filtered off
  5. customdried
  6. customThe crude solid was recrystallised from ethanol (110 ml)

Quellen und Nachweise

ORD-Eintrag
ord-ab2c162a34bf498bb78f99e8c967b79e
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04894369

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