Dimethylamine → HCID 12668361, compound
Reaction equation
CNCCNCCNC.CNC.[CH3:13][N:14]([CH3:22])[P:15]([N:19]([CH3:21])[CH3:20])[N:16]([CH3:18])[CH3:17]>>[CH3:13][N:14]1[CH2:22][CH2:21][N:19]2[P:15]1[N:16]([CH3:18])[CH2:17][CH2:20]2Participants
Conditions
- Temperature
- 125 °C
Procedure
A mixture of 5.00 g of 1,7-dimethyldiethylenetriamine and 6.22 g of hexamethylphosphorous triamide is heated to 80° C, at which temperature dimethylamine begins to be evolved. Evolution of dimethylamine continues for about one hour, during which time the temperature is gradually raised to 125° C. The mixture is distilled to give 5.75 g (95%) of 2,8-dimethyl-2,5,8-triaza-1-phosphabicyclo[3.3.0]octane as a clear, colorless liquid, which boils at 55°-65° C at 0.30 mm. The nuclear magnetic-resonance spectrum (C6D6 /TMS) of the product shows a highly split pattern from δ 2.0 to 4.5 and has the expected sharp doublet for the --CH3 groups at δ 2.55, J = 10 Hz. The infrared absorption spectrum (neat) has absorptions at 3.5, 6.83, 6.91, 7.65, 7.80, 8.20, 8.68, 9.20, 9.70, 10.15, 10.4, 10.7, and 11.5 μ.
Workup
- distillationThe mixture is distilled
Sources & evidence
- ORD record
- ord-e14c8f900a3c47189fce595e95fcab9c
- Source dataset
- uspto-grants-1976_12
- Patent number
- US03996276
Reaction notes
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