Hydrochloric Acid → 6-{1-Hydroxy-4-[bis-chloroethyl-amino]butyl}-3,4-dihydrocarbostyril

HRID 1285441Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1285441
[O:1]=[C:2]([C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[NH:19][C:18](=[O:23])[CH2:17][CH2:16]2)[CH2:3][CH2:4][CH2:5][N:6]([CH2:10][CH2:11][Cl:12])[CH2:7][CH2:8][Cl:9].[BH4-].[Na+].Cl.[OH-].[Na+]>CO.O>[OH:1][CH:2]([C:13]1[CH:14]=[C:15]2[C:20](=[CH:21][CH:22]=1)[NH:19][C:18](=[O:23])[CH2:17][CH2:16]2)[CH2:3][CH2:4][CH2:5][N:6]([CH2:10][CH2:11][Cl:12])[CH2:7][CH2:8][Cl:9]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 202294206-{1-Oxo-4-[di-(2-chloroethyl)-amino]butyl}-3,4-dihydrocarbostyril

Produkt 1

HCID 202294566-{1-Hydroxy-4-[bis-chloroethyl-amino]butyl}-3,4-dihydrocarbostyril

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

2.5 Grams of 6-{1-oxo-4-[di-(2-chloroethyl)-amino]butyl}-3,4-dihydrocarbostyril was dissolved in 80 ml of methanol, with stirring at a room temperature condition 1.6 g of sodium borohydride was added gradually to the mixture in 15 minutes and further stirred at a room temperature for 2 hours. To the reaction mixture was added 5 ml of concentrated hydrochloric acid was added and the reaction mixture was concentrated under a reduced pressure to dryness. The residue thus obtained was dissolved in 10 ml of water, the pH of the solution was adjusted to 6-7 by adding 2N-sodium hydroxide aqueous solution and stirred to precipitate crystals. The crystals were collected by filtration washed with water and dried to obtain 1.4 g of 6-{1-hydroxy-4-[bis(2-chloroethyl)amino]-butyl}-3,4-dihydrocarbostyril in colorless powdery product.

Aufarbeitung

  1. additionwas added gradually to the mixture in 15 minutes
  2. additionwas added
  3. concentrationthe reaction mixture was concentrated under a reduced pressure to dryness
  4. customThe residue thus obtained
  5. stirringstirred
  6. customto precipitate crystals
  7. filtrationThe crystals were collected by filtration
  8. washwashed with water
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-382d5b18491a49d0a5dc794474c55aed
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04567187

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