申请人:Ciba Specialty Chemicals Holding Inc.
公开号:EP1116714A1
公开(公告)日:2001-07-18
There is disclosed an improved process for the preparation of a compound of the formula I
wherein n is 0 or 1, R1 is C1-C12alkyl or -CH2SR3, R2 is C1-C12alkyl, C7-C9phenylalkyl, C7-C9-phenylalkyl substituted on the phenyl radical by from 1 to 3 C1-C4alkyl groups; or -CH2SR3, R3 is C6-C18alkyl, phenyl or benzyl, R4 is hydrogen or methyl, R5 is hydrogen or methyl, with the proviso that R4 and R5 are not simultaneously methyl, by reacting a compound of the formula II
wherein n, R4 and R5 are as previously defined, R11 is hydrogen or C1-C12alkyl; and R12 is hydrogen, C1-C12alkyl, C7-C9phenylalkyl, C7-C9phenylalkyl substituted on the phenyl radical by from 1 to 3 C1-C4alkyl groups; with formaldehyde or a compound that liberates formaldehyde under the reaction conditions and with at least one compound of the formula III
R3SH (III)
wherein R3 is as previously defined, in the presence of a base, said base being mono- or dimethylamine or mono- or diethylamine, which process comprises treating afterwards the reaction product with a reducing agent.
本发明公开了一种制备式 I 化合物的改进工艺
其中 n 为 0 或 1,R1 为 C1-C12 烷基或-CH2SR3,R2 为 C1-C12 烷基、C7-C9 苯基、在苯基上被 1 至 3 个 C1-C4 烷基取代的 C7-C9 苯基;或-CH2SR3,R3 为 C6-C18 烷基、苯基或苄基,R4 为氢或甲基,R5 为氢或甲基,但 R4 和 R5 不同时为甲基,通过反应式 II 的化合物来制备。
其中 n、R4 和 R5 如前所定义,R11 是氢或 C1-C12烷基;R12 是氢、C1-C12烷基、C7-C9 苯基、苯基上被 1 至 3 个 C1-C4 烷基取代的 C7-C9 苯基;与甲醛或在反应条件下能释放甲醛的化合物以及至少一种式 III 的化合物进行反应
R3SH (III)
其中 R3 如前定义,在碱存在下,所述碱为一甲胺或二甲胺或一乙胺或二乙胺,该过程包括随后用还原剂处理反应产物。