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list of experiments
Solubility book (3rd Edn)
Hai Truong and Khalid Mirza
To study the effect of n-butyl isocyanide on the solubility of the Ugi product UCExp176C in benzene.
Saturated solution of the Ugi product UC176C in benzene spiked with butylisocyanide was prepared in three one dram vials by adding 20uL, 40uL and 60uL of isocyanide the vials. These vials along with two blank (unspiked) solution were placed in a 40C water bath for 24h. They were then left for another 24h at 25C to equilibrate. The supernatants from each vial was separated and HNMR inconjunction with SAMS was used to calculate the solutbility of the Ugi product in the solution.
It is obvious from the
that there is a negligible effect of isonitrile on the solubility of the Ugi product UC176C.
No effect of the isocyanide concentration was observed on the solubility of the Ugi product UC176C
15:32 Prepared 5 half-dram vials. Label from Exp158-1, Exp158-2, Exp158-3, Exp158-4, and Exp158-5. Under a hood, put 300uL of benzene into each vials.
15:40 Put Ug176C into each vial and vortexed for 15 seconds for each to be sure there was still solid remained in the solution of each vials.
15: 50 Under the hood, put n-butyl isocyanide into each vial as following amount:
Vial Exp158-1: 20uL
Vial Exp158-2: 40uL
Vial Exp158-3: 60uL
Vial Exp158-4: zero (blank solution)
Vial Exp158-5: zero (blank solution)
16:15 Parafilmed all vials.
16:45 Put them into Lauda heating/cooling bath. Temperature in the bath was 27C. Adjusted temperature to 40C.
14:20 Changed the setting on the water/glycol bath to 25C, the actual temperature was at 40C.
20:30 Removed the vials from the bath. Centrifuged the vials. The temperature of the bath was at 25C
21:05 In to five clean/dry NMR tubes, pipetted out DMSO-d6 (~500uL) and labeled the tubes ONSCExp158-1A and ONSCExp158-2A, ONSCExp158-3A, ONSCExp158-4A, ONSCExp158-5A.
21:10 Transferred approximately 200uL of the supernatant from each vial in to the corresponding NMR tubes.
22:30 Obtained HNMRs of ONSCExp158-1A-1 through ONSCExp158-12A
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