Water → 1-{[(1H-1,2,3-benzotriazol-1-ylmethyl)sulfanyl]methyl}-1H-1,2,3-benzotriazole

HRID 487845

Reaktionsgleichung

Reaktionsgleichung von HRID 487845
Cl[CH2:2][N:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[N:4]1.O.[S-2:13].[Na+].[Na+].O>C(O)C>[N:3]1([CH2:2][S:13][CH2:2][N:3]2[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[N:5]=[N:4]2)[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[N:4]1

Komponenten

5

Edukt 3

HCID 962WaterHCID 33282221-(Chloromethyl)-1H-benzotriazoleHCID 19906495Sodium sulfide monohydrate

Produkt 1

HCID 37660921-{[(1H-1,2,3-benzotriazol-1-ylmethyl)sulfanyl]methyl}-1H-1,2,3-benzotriazoleAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1-(Chloromethyl)benzotriazole (20.4 g), prepared above, and sodium sulfide monohydrate (14.4 g) in anhydrous ethanol (75 ml) were stirred overnight (20 hours) at room temperature. Water (240 ml) was added to the reaction mixture. The precipitate was filtered, washed with water to remove inorganic salts and dried. Crystallization from ethanol gave 15.6 g (88%) of desired product (Compound 1); m.p. 179°-181° C. (lit. 182°-184° C.). Thin Layer Chromotography in (CHCl3 /Ethyl acetate) showed only one spot.

Aufarbeitung

  1. filtrationThe precipitate was filtered
  2. washwashed with water
  3. customto remove inorganic salts
  4. customdried
  5. customCrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-21d61f07ab5e409ea3eec212aa4b057a
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05298390

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