Iodine → GDMA 3-methyl-3-butene-1-ol
반응식
[CH2:1]([O:8][C:9]([CH2:11][SH:12])=[O:10])[CH2:2][O:3][C:4]([CH2:6][SH:7])=[O:5].[CH3:13][C:14](=[CH2:18])[CH2:15][CH2:16][OH:17].II>>[CH2:2]([O:3][C:4]([CH2:6][SH:7])=[O:5])[CH2:1][O:8][C:9]([CH2:11][SH:12])=[O:10].[CH3:18][C:14](=[CH2:13])[CH2:15][CH2:16][OH:17]참가 물질
4
반응 조건
- 온도
- 60 °C
실험 절차
The flask was set up for reaction and agitation as described in Example 6. No heat was initially added to the flask containing the GDMA. The addition funnel containing the 3-methyl-3-butene-1-ol was placed on the second neck of the flask and a slow drip was started. The reaction exotherm was mild and the addition was completed in 40 minutes. The flask was then heated to 60° C. and held for one hour. Iodine titration indicated a significant amount of free thiol remaining (3.72 meq/g). Lupersol 575 (2.5 g) was added slowly. A significant exotherm occurred, after which the free thiol was measured to be 0.047 meq/gram. The material was then stored in dark high density polyethylene bottles.