Hydrazine hydrate (1:1) → HCID 178514365, compound

HRID 431497Notes

Reaction equation

HRID 431497 reaction equation
[NH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[N:4]=[N:3][C:2]1=S.O.[NH2:16][NH2:17]>>[NH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[N:4]=[N:3][C:2]1=[N:16][NH2:17]

Participants

3

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 178527928HCID 178527928, compound

Product 1

HCID 178514365HCID 178514365, compound

Conditions

Temperature
120 °C

Procedure

A solution of 1,9-Dihydro-1,3,4,9-tetraaza-fluorene-2-thione 14c (56 mmol, 1 equiv.) in hydrazine hydrate (195 mL) is heated to reflux (120° C.) for 4 hours as disclosed in Joshr, K. C.; Dandia, A.; Bawbia, S. J. Ind Chem. Soc. (1989), 66, 690-693 and references therein. The mixture is allowed to cool to room temperature for 48 hours. The orange-yellow precipitate is filtered, washed with water and ethanol, and dried under vacuum for 15 hours to yield (1,9-Dihydro-1,3,4,9-tetraaza-fluoren-2-ylidene)-hydrazine 14d as a yellow powder.

Workup

  1. temperatureto cool to room temperature for 48 hours
  2. filtrationThe orange-yellow precipitate is filtered
  3. washwashed with water and ethanol
  4. customdried under vacuum for 15 hours

Sources & evidence

ORD record
ord-a3c506a45eb34a8a88a8e356019e9fb5
Source dataset
uspto-grants-2003_12
Patent number
US06660737B2

Reaction notes

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