Sodium Hydroxide → Crisnatol

HRID 1193716

Reaktionsgleichung

Reaktionsgleichung von HRID 1193716
Cl.[CH:2]1[C:19]2[CH:18]=[CH:17][C:16]3[C:7](=[CH:8][C:9]([CH2:20][NH:21][C:22]([CH3:27])([CH2:25][OH:26])[CH2:23][OH:24])=[C:10]4[C:15]=3[CH:14]=[CH:13][CH:12]=[CH:11]4)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO.O>[CH:2]1[C:19]2[CH:18]=[CH:17][C:16]3[C:7](=[CH:8][C:9]([CH2:20][NH:21][C:22]([CH3:27])([CH2:23][OH:24])[CH2:25][OH:26])=[C:10]4[C:15]=3[CH:14]=[CH:13][CH:12]=[CH:11]4)[C:6]=2[CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 133752782-((6-Chrysenylmethyl)amino)-2-methyl-1,3-propanediol hydrochloride

Produkt 1

HCID 57062CrisnatolAusbeute 96,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a rapidly stirred solution of 2-((6-chrysenylmethyl)amino)-2-methyl-1,3-propanediol hydrochloride (1B, 20 g, 52.36 mmol) in a mixture of CH3OH (200 mL) and H2O (800 mL) was added dropwise over 10 min a 1N NaOH solution (55 mL). The resulting white precipitate was filtered and washed with warm H2O (4×500 mL) and then with Et2O (1 L), sucked dry and placed in a vacuum oven overnight. A total of 17.43 g (96.4%) of 2-((6-chrysenylmethyl)amino)-2-methyl-1,3-propanediol mp 200°-202°, (C,H,N) was obtained.

Aufarbeitung

  1. filtrationThe resulting white precipitate was filtered
  2. washwashed with warm H2O (4×500 mL)
  3. dry with materialwith Et2O (1 L), sucked dry
  4. customplaced in a vacuum oven overnight

Quellen und Nachweise

ORD-Eintrag
ord-bc0a9da6ad1045009db5300c319d950d
Quelldatensatz
uspto-grants-1989_03
Patentnummer
US04810727

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