tert-Butylhydrazine → HCID 21431129, compound

HRID 436738Notes

Reaction equation

HRID 436738 reaction equation
[C:1]([N:5]=[N:6][C:7]1([N:13]=[C:14]=[S:15])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([CH3:4])([CH3:3])[CH3:2].[C:16]([NH:20][NH2:21])([CH3:19])([CH3:18])[CH3:17]>CCCCC>[C:1]([N:5]=[N:6][C:7]1([NH:13][C:14](=[S:15])[NH:21][NH:20][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1)([CH3:4])([CH3:2])[CH3:3]

Participants

4

Reactant 2

HCID 81890tert-ButylhydrazineHCID 214311441-t-Butylazo-1-isothiocyanatocyclohexane

Product 1

HCID 21431129HCID 21431129, compound

Reagents, catalysts & solvents 1

HCID 8003PentaneSolvent2×

Procedure

To 8.7 grams (.0376 moles) of 1-t-butylazo-1-isothiocyanatocyclohexane cooled to 5° C. and stirred with a magnetic stirrer in a 50 ml erlenmeyer flask was added dropwise 4.36 grams (.0376 moles) of a 76% aqueous solution of t-butylhydrazine. The reaction was very exothermic and rapid and was complete almost immediately after the addition was complete. Pentane was added to slurry up the solids and the mixture stirred for 1 hour at room temperature. The pentane was stripped from the reaction mixture to leave a yellow solid weighing 11.3 grams (94.5% crude yield). The product melted at 120°-122° C. and the infrared spectrum of the product had sharp strong bands at 1540 and 1520 cm-1 and sharp NH bands at 3150 and 3280 cm-1.

Workup

  1. additionafter the addition
  2. stirringthe mixture stirred for 1 hour at room temperature
  3. customto leave a yellow solid

Sources & evidence

ORD record
ord-3346bb515c1a4bc1a4c8a769064b83a8
Source dataset
uspto-grants-1977_06
Patent number
US04028344

Reaction notes

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