Hydrazine hydrate (1:1) → HCID 13037944, compound

HRID 1660320Notes

Reaction equation

HRID 1660320 reaction equation
[CH3:1][C:2]1([CH3:13])[O:6][CH:5]([CH2:7][NH:8][C:9](=S)[S:10]C)[CH2:4][O:3]1.O.[NH2:15][NH2:16]>C(O)C>[CH3:1][C:2]1([CH3:13])[O:6][CH:5]([CH2:7][NH:8][C:9](=[S:10])[NH:15][NH2:16])[CH2:4][O:3]1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 54240341HCID 54240341, compound

Product 1

HCID 13037944HCID 13037944, compoundYield 69.4%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of methyl N-(2,2-dimethyl-dioxolan-4-yl-methyl)-dithiocarbamate (23,6 g) prepared according to U.S. Pat. No. 4,064,242, absolute ethanol (500 cc) and hydrazine hydrate (5.6 g) is heated under reflux for 2 hours 30 minutes. It is then concentrated to dryness at 20° C. under 20 mm Hg (2.7 kPa) and the residue is taken up in diethyl ether (100 cc). After filtration and drying, 4-(2,2-dimethyl-dioxolan-4-yl-methyl)-thiosemicarbazide (15.2 g) is obtained in the form of a cream-coloured solid melting at 145° C.

Workup

  1. customprepared
  2. temperatureunder reflux for 2 hours 30 minutes
  3. concentrationIt is then concentrated to dryness at 20° C. under 20 mm Hg (2.7 kPa)
  4. filtrationAfter filtration
  5. customdrying

Sources & evidence

ORD record
ord-45f1211180ea472db7d7d00328d45c10
Source dataset
uspto-grants-1981_12
Patent number
US04307116

Reaction notes

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