反应 #3482118
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US03959509
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a refluxing mixture of methanol (30 cc) and diethyl amine (15 cc) at 59°C is added 0.8 grams of threo-3-mercapto-2-butanol produced according to Example II and 0.3 grams of cis-2,3-butane episulfide produced according to Example III (0.3 grams). The reaction mass is refluxed for a period of 5 hours at 59°-64°C, after which time it is allowed to remain at room temperature overnight. The reaction mass is then reheated to 61°C and allowed to remain at that temperature for a period of 3 hours after which GLC analysis indicated that most of the starting material is reacted. The major product is isolated via GLC (same conditions as Example VII) and analyzed via mass spectral, NMR and IR analyses to be the threo-threo 3((2-mercapto-1-methylpropyl) thio)-2-butanol having the structure: ##SPC23## produced produced The reaction mass is refluxed for a period of 5 hours at 59°-64°C is then reheated to 61°C to remain at that temperature for a period of 3 hours is reacted The major product is isolated via GLC (same conditions as Example VII)
来源 ID: ord-1c10b5ac865a4a0d9170cb4ce09d52a0