Overview | tetrahydropyran-4-hydrazine Dihydrochloride is useful as an intermediate in organic synthesis. If tetrahydropyran-4-hydrazine Dihydrochloride is inhaled, move the patient to fresh air; If skin contact occurs, remove contaminated clothing and thoroughly rinse the skin with soap and water, if there is discomfort, medical treatment; If the eyes contact, should separate the eyelids, with running water or saline rinse, and immediately seek medical treatment; If you eat, immediately gargle, prohibit vomiting, should immediately seek medical treatment. |
preparation | the target compound tetrahydropyran-4-hydrazine dihydrochloride was prepared from anhydrous hydrazine and p-chloro-Tetrahydropyran as starting materials. Experimental procedure: Synthesis of anhydrous hydrazine hydrazine hydrate (25g, 80% mol) was added to a 0.40 ml round bottom flask, followed by potassium hydroxide (10g,0.17 mol), after standing overnight at 0 °c, the supernatant was transferred to another round-bottom flask and sodium hydroxide (21g,0.53 mol) was added and purged with argon, reflux under the condition of isolated air for 2 hours, check the reaction progress by thin layer chromatography, after the reaction is finished, cool down, atmospheric distillation, collect 114-116 ℃ fraction, 9.6g of anhydrous hydrazine, a colorless fuming liquid with an amine odor, was obtained in a yield of 75%. Synthesis of tetrahydropyran-4-hydrazine dihydrochloride anhydrous hydrazine (9.6g,300 mmoI) was added into a 250 mL three-necked flask under argon atmosphere, add freshly distilled p-chloro-Tetrahydropyran (21.6g,200 mmoI), stir for 1 hour, stir overnight at room temperature, check the progress of the reaction by TLC, after completion of the reaction, stand still, after rapid filtration in argon atmosphere, the filtrate was subjected to vacuum distillation under oxygen-free conditions, and fractions (250) at 55-57 °c were collected, tetrahydropyran-4-hydrazine dihydrochloride was obtained as a colorless transparent liquid in a yield of 14.6g and 83%. |