HRID845224
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 5.3 g (0.03 mole) of 1-(chloromethyl)naphthalene and 8.6556 g (0.033 mole) of triphenylphosphine in 150 mL of dimethylformamide was heated at reflux with stirring for 5 hours. A copious white precipitate formed. The precipitate was filtered and washed with 100 mL of dimethylformamide and 100 mL of ether. The product was dried in vacuo to yield 11.97 g (91%) of 1-naphthylmethyltriphenylphosphonium chloride as white crystals: mp 285°-288°; IR (KBr) 3050, 3010, 2880, 2790, 1665, 1590, 1510, 1485, 1440, 1385, 1335, 1275, 1155, 1110, 1095, 875, 810, 785, 730, and 690 cm-1 ; NMR (DMSO) δ5.67 (d, J=15 Hz, 2H), 7.60 (m, 15H) and 7.73 (m, 7H).
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux
- customA copious white precipitate formed
- filtrationThe precipitate was filtered
- washwashed with 100 mL of dimethylformamide and 100 mL of ether
- customThe product was dried in vacuo