chlorosulfanyl thiohypochlorite

实验步骤: 投料: 在250ml 三口瓶中加入4.73g SM、120ml DCM，滴入3~4滴TEA助溶，置换N2后针筒注入1.70ml（1.2eq）TEA，干冰乙醇浴中冷却至外温-30℃保持15min（保证内温在-20℃以下），再缓慢滴入0.5ml（0.6eq）Cl2S2，外温-30℃下保持30min。\n监测: LCMS（165010-1-3-R-30min）监测原料已消耗完全，产物峰较干净。\n后处理: 反应液转至冰水浴中，缓慢注入60ml H2O淬灭反应，冰水浴中搅拌1h。1h后倒出反应液加入100ml DCM，100ml H2O萃取，收集有机相浓缩。\n监测: TLC（纯EA, EA:DCM=1:1）监测纯EA时产物Rf=0.85，上方有个极性小的杂质点与产物分离度并不大，但换成展开剂EA:DCM=1:1时，杂质爬顶，产物Rf不变。\n纯化: 旋干的粗品加入20ml DCM、100ml EA，用棍子捣碎至无颗粒状后超声打浆15min过滤，用EA洗涤滤饼数次，送检数据HNMR有残留EA，加水冻干，HPLC纯度96.8%，入库4.00g白至类白色粉末。

实验步骤: 投料: 准备50ml 双口瓶中加入234mg SM、5ml DCM，置换N2后针筒注入0.08ml（1.2eq）TEA，干冰乙醇浴冷却至-20℃再缓慢滴入0.04ml（0.6eq）Cl2S2，保持-20℃搅拌反应。\n后处理: 反应体系加入5ml 纯水淬灭，加入DCM萃取，收集有机相浓缩，送检LCMS（165010-1-2-Lv）均已反应完全，HPLC确定有明显杂质峰，后续生产减少反应时间进行监测。

实验步骤: 投料: 准备50ml 双口瓶中加入234mg SM、5ml THF，置换N2后针筒注入0.08ml（1.2eq）N-甲基吗啉溶清，冰浴冷却至0℃再缓慢滴入0.04ml（0.6eq）Cl2S2，保持冰浴搅拌反应。\n后处理: 反应体系加入5ml 饱和食盐水淬灭，加入DCM萃取，收集有机相浓缩，送检LCMS（165010-1-1-Lv）均已反应完全，HPLC确定有明显杂质峰，后续生产减少反应时间进行监测。

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 4.6 g (34 mmol) of aluminum chloride and 4.6 g (34 mmol) of disulphur dichloride in 344 g (2.55 mol) of sulphuryl chloride was added dropwise to a mixture of 57.5 g (250 mmol) of p-chlorobenzotrichloride and 115 g (850 mmol) of sulphuryl chloride at 40° C. The reaction mixture was further processed in the manner described in Example 5, that is to say that, after the working up, unreacted p-chlorobenzotrichloride and 3,4-dichlorobenzotrichloride were separated off by distillation and fed to renewed chlorination with sulphuryl chloride under the conditions given here. By distillation of the combined sump fractions, 2,4,5-trichlorobenzotrichloride was obtained in a yield of 47% of theory. were separated off by distillation and fed By distillation of the combined sump fractions