Page 226 - 《精细化工》2022年第9期
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·1944·                            精细化工   FINE CHEMICALS                                 第 39 卷

            总摩尔收率可达~38%。本工艺具有如下特点:                             [9]   LU W Q, YU W W, HE J C, et al. Reprogramming immunosuppressive
                (1)(S/R)-1-苯乙胺氨基上保护基与苯环对位溴                         myeloid cells facilitates immunotherapy for colorectal cancer[J].
            代一锅法反应中,保护基选择三氟乙酰基,对于后                                 EMBO Molecular Medicine, 2021, 13(1): 12798.
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                                                                   pharmacophore modeling and in vitro activity of 10,11-dihydrodibenzo
            好的兼容性;在(0±2)℃下,当投料比为 n(DBDMH)/
                                                                   [b,f]oxepine-4-carboxamide derivatives as novel and potent antagonists
            n(Ⅱ)=0.55 时,可获得摩尔收率为 50.7%的对位溴代                        of the prostaglandin EP4 receptor[J]. Bioorganic &  Medicinal
            产物Ⅲ;粗产品根据杂质实际情况,采用 V(无水甲                               Chemistry Letters, 2011, 21(21): 6336-6340.
            醇)/ V(水)=1 体系作为重结晶溶剂,可有效去除副产                       [11]  ELENA C, FRANCESCO C,  TERESA D,  et al. Heterocondensed
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            收率及产品质量都较稳定。                                           WO2019224096A1[P]. 2019-11-28.
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            度、正丁基锂用量对苯基对位甲酸化反应的影响,                             [13]  ZHANG S W, GONG C J, SU M B, et al. Synthesis and in vitro and
            当投料比为 n(Ⅲ)∶n(正丁基锂)=1∶2.0,反应温度                          in vivo biological  evaluation  of tissue-specific bisthiazole histone
            低于–60  ℃,摩尔收率最高达到 90.9%,且工艺及                           deacetylase (HDAC) inhibitors[J]. Journal  of Medicinal  Chemistry,
            收率稳定。                                                  2020, 63(2): 804-815.
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            下一步完成羧基甲酯化和脱保护基,然后再对氯化亚
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            砜用量及反应温度进行优化,在 65  ℃下,投料比为                             WO2001074391A1[P]. 2001-10-11.
            n(Ⅳ)∶n(氯化亚砜)=1∶3.0,摩尔收率可达 84.1%。                   [16]  MAKOTO  N, HAJIME N, MASAYOSHI U. Preventives/remedies
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            便,总摩尔收率高达~38%,e.e.值>99%。
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