反应 #6706

ord-b168db1e34b1403f93a8212f0332cfb6

反应方程式

C=CCCCCC(C)[Si](C)(C)Cl
7-oct-1-enyldimethylchlorosilane
CCN(CC)CC
triethylamine
O
water
C=CCCCCC(C)[Si](C)(C)O
7-oct-1-enyldimethylsilanol

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤filtered
  2. 2
    洗涤washing the filtered solid with ether (10 ml)
  3. 3
    其他The filtrate was evaporated with a rotary evaporator
  4. 4
    其他the residue partitioned between hexane (30 ml) and water (30 ml)
  5. 5
    其他The organic layer was separated
  6. 6
    干燥dried (MgSO4)
  7. 7
    过滤filtered through silica gel (70–230 mesh, 60 Å)
  8. 8
    洗涤washing with hexane (100 ml)
  9. 9
    其他The filtrate was evaporated with a rotary evaporator
  10. 10
    其他to afford a colorless oil which
  11. 11
    其他dried

实验过程

A solution of 7-oct-1-enyldimethylchlorosilane (2.56 ml) in ether (2 ml) was added dropwise over 1 hour to a stirring mixture of triethylamine (1.5 ml), water (0.18 ml) and ether (15 ml) in an ice/water bath. The resultant was stirred a further 1 hour in the ice/water bath and filtered washing the filtered solid with ether (10 ml). The filtrate was evaporated with a rotary evaporator and the residue partitioned between hexane (30 ml) and water (30 ml). The organic layer was separated, dried (MgSO4) and filtered through silica gel (70–230 mesh, 60 Å), washing with hexane (100 ml). The filtrate was evaporated with a rotary evaporator to afford a colorless oil which was vacuum dried and weighed (1.06 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07083984B2uspto-grants-2006_08