1 1,3,5-Triformylbenzene (32.4 mg, 0.2 mmol) and 2,5-dimethoxyterephthalohydrazide (76.3 mg, 0.3 mmol) were added to a pyrex tube. To the mixture were added mesitylene (6 mL), anhydrous dioxane (2 mL), and aqueous acetic acid (6m, 0.8 mL). The tube was immersed in an ultrasonic bath for 10 min. The mixture was then degassed through three freeze–pump–thaw cycles, sealed under vacuum. After warming to room temperature, the sealed tube was placed in an oven at 1208C and left undisturbed for 3 days, yielding a pale-yellow solid. The solid was ChemSusChem 2017, 10, 664 – 669 三甲苯：二氧六环：乙酸（6M） =15:5:2 BET=1501 isolated by filtration and washed with anhydrous THF and anhydrous acetone. The resulting solid was dried under vacuum at 608C for 12 h to afford the COF as a pale-yellow powder (96.7 mg, 89% yield). 2 Synthesis of COF-43. Dihydrazide 1 (37.0 mg, 0.131 mmol) and trialdehyde 2 (34.0 mg, 0.087 mmol) were sonicated in 1 mL mesitylene / dioxane (9:1 v/v) in a 4 mL vial until a fine suspension was obtained. The suspension was then transferred by pipet to a pre-scored 5 mL ampoule, 6 M acetic acid (0.1 mL) was added, and the whole mixture was flash frozen in N2 (l) and flame sealed. The ampoule was put in an oven at 120 °C for 72 h, after which the ampoule was cooled to rt, opened, and the solvent was removed with a pipette. THF (2 mL) was added, and after 1 h, the solvent was removed with a pipette. This THF activation process was then 溶剂剥层 repeated to provide COF-43 as an insoluble microcrystalline powder. J. Am. Chem. Soc. 2013, 135, 14952−14955三甲苯：二氧六环：乙酸（6M） =9:1:1 3 A 4 mL pyrex tube was charged with triformylphloroglucinol (30 mg, 0.14 mmol), 2,5-dimethoxyterephthalohydrazide (54 mg, 0.21 mmol), mesitylene/dioxane (2 mL, 3:1 v/v) and AcOH (0.2 mL, 6 M), the mixture was sonicated for 1 minutes, degassed through three freeze–pump–thaw cycles, sealed under vacuum. The reaction was heated at 120 ºC for 7 days yielding a pale-yellow solid at the bottom of the tube which was isolated by centrifugation and washed with anhydrous dioxane, anhydrous tetrahydrofuran and anhydrous acetone, and dried under vacuum at 50 °C for 10 h to afford pale yellow powder 67.4 mg in 84% isolated yield Chem. Commun., 2016, 52, 三甲苯：二氧六环：乙酸（6M） =15:5:211088--11091 4 To a Biotage® 5 mL microwave vial 17.7 mg (0.044 mmol, 2.0 eq.) of TFPT (1) and a stir bar was added. Then 18.6 mg (0.066 mmol, 3.0 eq.) of 2,5-diethyoxy-terephthalohydrazide was added and the vial was temporally sealed with a rubber septum. Subsequently, the vial was flushed three times in argon/vacuum cycles. To the mixture 0.66 mL of mesitylene and 0.33 mL of 1,4-dioxane were added and again degassed three times in argon/vacuum cycles. In one shot 100 μL aqueous 6M acetic acid was added, the vial was sealed and heated in a stirred oil bath with 120 °C (preheated) on a heating stirrer for 72 h. After slow cooling to room temperature the vial was opened and the whole mixture was centrifuged (3 x 15 min, 20000 rpm) Chem. Sci., 2014, 5, 三甲苯：二氧六环：乙酸（6M） 2789–2793 =2:1:1.66 while being washed with DMF (1 x 7 mL) and THF (2 x 7 mL). The resulting yellow precipitate was transferred to a storage vial with DCM, dried at room temperature, then in vacuum and characterized by powder X-ray diffraction. 5 Synthesis of COF-AO (1). A 1,4-dioxane/mesitylene (1.5/4.5 mL) solution of 2,5-bis(allyloxy)terephthalohydrazide (46 mg, 0.15 mmol), triformylphloroglucinol (21 mg, 0.1 mmol), and acetic acid (0.6 mL, 6.0 M) in a pyrex tube was flash frozen in a liquid nitrogen bath and degassed. Upon warming to room temperature, the tightly capped tube was heated at 120 °C for 3 days. The obtained precipitate was collected by centrifugation and completely washed with acetone and ethanol, separately. The collected solids were dried in vacuum to generate the ACS Mater. Appl. 三甲苯：二氧六环：乙酸（6M） =15:5:2Interfaces 2018, 10, 2045720448− as-synthesized COF-AO (1) as yellow crystalline solids (51 mg, 75% yield). 6 397.11 m2/g. J. Mater. A, 6, 三甲苯：二氧六环：乙酸（6M） =15:5:2 Synthesis of TpTe-1. Terephthalohydrazide (0.15 mmol) and 1,3,5-triformylphloroglucinol (0.10 mmol, Tp) were weighed into a glass pressure tubing. After addition of 1,4-dioxane (1.0 mL), mesitylene (3.0 mL), and 0.4 mL of 6.0 M aqueous acetic acid, the tube was then flash frozen at 77 K (liquid N2 bath) and degassed by three freeze-pump-thaw cycles. The tube was sealed off and then heated at 120 °C for 3 days. A yellow colored precipitate was isolated by BET:350 centrifugation and washed with acetone (3×10 mL) and THF (3×10 mL), dried at 80 °C under vacuum for 24 h to yield TpTe-1 as yellow powder in 80 % yield. Chem. 2018, 11140–11146