Cyclohexylisopropylamine → HCID 123933952, compound
Reaction equation
[CH:1]([NH:4][CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)([CH3:3])[CH3:2].C(N([SiH3:18])C(C)C)(C)C>>[CH:1]([N:4]([SiH3:18])[CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1)([CH3:3])[CH3:2]Participants
3
Procedure
In a 500 ml Schlenk flask 247.3 g (1.75 mol) N-isopropylcyclohexylamine and 229.9 g (1.75 mol) di-isopropylaminosilane were refluxed for 8 days under nitrogen. The byproduct di-isopropylamine was removed with vacuum at a pressure of 40 mmHg and 50° C. Fractional vacuum distillation provided 50 g of pure N-isopropylcyclohexylaminosilane. The normal boiling point (measured at 1 atmosphere) is about 199° C. measured by differential scanning calorimetry (DSC). The end-product was characterized by mass spectroscopy (MS) which is provided in FIG. 1 with peaks at 171 (M+), 156 (M-CH3).
Workup
- customThe byproduct di-isopropylamine was removed with vacuum at a pressure of 40 mmHg and 50° C
- distillationFractional vacuum distillation
Sources & evidence
- ORD record
- ord-94b580ecd12f48168c52e1cda11d5a03
- Source dataset
- uspto-grants-2014_07
- Patent number
- US08771807B2
Reaction notes
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