R.
|
Solvent
|
Temp
(ÂșC)
|
Proportion Solv.
(g:g)
|
Stage
*3x (g)
|
Reaction Time (min)
|
Reaction Time (min)
|
Reaction Time (min)
|
Carbon
Amount
(%)*
|
|
|
|
|
|
t1
|
t2
|
t3
|
|
1 |
NaOH |
r.t |
20:1 |
|
90 |
- |
- |
21.03 |
2 |
NaOH |
r.t |
20:1 |
|
90 |
- |
- |
18.18 |
3 |
Hexane |
r.t |
20:1 |
|
90 |
- |
- |
8.69 |
4 |
Hexane |
r.t |
20:1 |
|
90 |
- |
- |
11.72 |
5 |
Hexane |
r.t |
15:1 |
*3x 5 |
30 |
30 |
30 |
9.74 |
6 |
Hexane |
50 |
15:1 |
*3x 5 |
30 |
30 |
30 |
9.20 |
7 |
Ethyl acetate |
r.t. |
15:1 |
*3x 5 |
30 |
30 |
30 |
5.72 |
8 |
Ethyl acetate |
50 |
15:1 |
*3x 5 |
30 |
30 |
30 |
5.66 |
9 |
THF |
r.t |
15:1 |
*3x 5 |
30 |
30 |
30 |
4.31 |
10 |
THF |
50 |
15:1 |
*3x 5 |
30 |
30 |
30 |
4.40 |
11 |
Ethanol |
r.t |
15:1 |
*3x 5 |
30 |
30 |
30 |
6.13 |
12 |
Dichloromethane |
r.t |
15:1 |
*3x 5 |
30 |
30 |
30 |
9.15 |
13 |
Acetonitrile |
r.t |
15:1 |
*3x 5 |
30 |
30 |
30 |
9.79 |
14 |
THF |
r.t |
30:1 |
*3x 10 |
30 |
30 |
30 |
3.89 |
15 |
THF |
r.t |
45:1 |
*3x 15 |
30 |
30 |
30 |
3.83 |
16 |
THF |
r.t |
60:1 |
*3x 20 |
30 |
30 |
30 |
3.75 |
17 |
THF |
r.t |
15:1 |
*3x 5 |
20 |
20 |
20 |
8.93 |
18 |
THF |
r.t |
15:1 |
*3x 5 |
10 |
10 |
10 |
8.14 |
19 |
THF |
r.t |
15:1 |
*3x 5 |
5 |
5 |
5 |
10.92 |