钆布醇杂质12 4HCl

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

实验步骤: To a suspension of tetraaza-12-crown-4 tetrahydrochloride (66.6 g, 0.209 mol, Parish, Inc.) in chloroform (2 L), was bubbled NH3 (g) through a gas dispersion tube for 1 hour. The solution was allowed to stir overnight and the white solid was filtered off and washed with CHCl3 (4×100 mL). The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) and dried under vacuum at ambient temperature. A second crop of the free base was isolated from the ether washes to give a combined yield of 35.1 g (97.5%). 1H NMR (CDCl3): δ 2.32 (s, 4 H), 2.70 (s, 16 H). was bubbled NH3 (g) through a gas dispersion tube for 1 hour the white solid was filtered off washed with CHCl3 (4×100 mL) The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) dried under vacuum at ambient temperature A second crop of the free base was isolated from the ether to give a combined yield of 35.1 g (97.5%)

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

实验步骤: To a suspension of tetraaza-12-crown-4 tetrahydrochloride (66.6 g, 0.209 mol, Parish, Inc.) in chloroform (2 L), was bubbled NH3 (g) through a gas dispersion tube for 1 hour. The solution was allowed to stir overnight and the white solid was filtered off and washed with CHCl3 (4×100 mL). The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) and dried under vacuum at ambient temperature. A second crop of the free base was isolated from the ether washes to give a combined yield of 35.1 g (97.5%). 1H NMR (CDCl3): δ 2.32 (s, 4 H), 2.70 (s, 16 H). was bubbled NH3 (g) through a gas dispersion tube for 1 hour the white solid was filtered off washed with CHCl3 (4×100 mL) The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) dried under vacuum at ambient temperature A second crop of the free base was isolated from the ether to give a combined yield of 35.1 g (97.5%)

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

实验步骤: 120.0 mg of cyclen tetrahydrochloride (1,4,7,10-tetraazacyclodecane tetrahydrochloride) and 100.0 mg of cucurbit[8]uril were dissolved in water. Heating followed by slow cooling of the solution produced an inclusion complex in which a cyclen molecule was encapsulated in the cavity of cucurbit[8]uril as a colorless crystalline material. Heating by slow cooling of the solution

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

实验步骤: 120.0 mg of cyclen tetrahydrochloride (1,4,7,10-tetraazacyclodecane tetrahydrochloride) and 100.0 mg of cucurbit[8]uril were dissolved in water. Heating followed by slow cooling of the solution produced an inclusion complex in which a cyclen molecule was encapsulated in the cavity of cucurbit[8]uril as a colorless crystalline material. Heating by slow cooling of the solution

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

实验步骤: 120.0 mg of cyclen tetrahydrochloride (1,4,7,10-tetraazacyclodecane tetrahydrochloride) and 100.0 mg of cucurbit[8]uril were dissolved in water. Heating followed by slow cooling of the solution produced an inclusion complex in which a cyclen molecule was encapsulated in the cavity of cucurbit[8]uril as a colorless crystalline material. Heating by slow cooling of the solution

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

实验步骤: To a suspension of tetraaza-12-crown-4 tetrahydrochloride (66.6 g, 0.209 mol, Parish, Inc.) in chloroform (2 L), was bubbled NH3 (g) through a gas dispersion tube for 1 hour. The solution was allowed to stir overnight and the white solid was filtered off and washed with CHCl3 (4×100 mL). The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) and dried under vacuum at ambient temperature. A second crop of the free base was isolated from the ether washes to give a combined yield of 35.1 g (97.5%). 1H NMR (CDCl3): δ 2.32 (s, 4 H), 2.70 (s, 16 H). was bubbled NH3 (g) through a gas dispersion tube for 1 hour the white solid was filtered off washed with CHCl3 (4×100 mL) The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) dried under vacuum at ambient temperature A second crop of the free base was isolated from the ether to give a combined yield of 35.1 g (97.5%)

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

实验步骤: To a suspension of tetraaza-12-crown-4 tetrahydrochloride (66.6 g, 0.209 mol, Parish, Inc.) in chloroform (2 L), was bubbled NH3 (g) through a gas dispersion tube for 1 hour. The solution was allowed to stir overnight and the white solid was filtered off and washed with CHCl3 (4×100 mL). The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) and dried under vacuum at ambient temperature. A second crop of the free base was isolated from the ether washes to give a combined yield of 35.1 g (97.5%). 1H NMR (CDCl3): δ2.32 (s, 4 H), 2.70 (s, 16 H). was bubbled NH3 (g) through a gas dispersion tube for 1 hour the white solid was filtered off washed with CHCl3 (4×100 mL) The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) dried under vacuum at ambient temperature A second crop of the free base was isolated from the ether to give a combined yield of 35.1 g (97.5%)

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

实验步骤: 120.0 mg of cyclen tetrahydrochloride (1,4,7,10-tetraazacyclodecane tetrahydrochloride) and 100.0 mg of cucurbit[8]uril were dissolved in water. Heating followed by slow cooling of the solution produced an inclusion complex in which a cyclen molecule was encapsulated in the cavity of cucurbit[8]uril as a colorless crystalline material. Heating by slow cooling of the solution

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

实验步骤: 120.0 mg of cyclen tetrahydrochloride (1,4,7,10-tetraazacyclodecane tetrahydrochloride) and 100.0 mg of cucurbit[8]uril were dissolved in water. Heating followed by slow cooling of the solution produced an inclusion complex in which a cyclen molecule was encapsulated in the cavity of cucurbit[8]uril as a colorless crystalline material. Heating by slow cooling of the solution

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

实验步骤: 120.0 mg of cyclen tetrahydrochloride (1,4,7,10-tetraazacyclodecane tetrahydrochloride) and 100.0 mg of cucurbit[8]uril were dissolved in water. Heating followed by slow cooling of the solution produced an inclusion complex in which a cyclen molecule was encapsulated in the cavity of cucurbit[8]uril as a colorless crystalline material. Heating by slow cooling of the solution

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

实验步骤: To a suspension of tetraaza-12-crown-4 tetrahydrochloride (66.6 g, 0.209 mol, Parish, Inc.) in chloroform (2 L), was bubbled NH3 (g) through a gas dispersion tube for 1 hour. The solution was allowed to stir overnight and the white solid was filtered off and washed with CHCl3 (4×100 mL). The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) and dried under vacuum at ambient temperature. A second crop of the free base was isolated from the ether washes to give a combined yield of 35.1 g (97.5%). 1H NMR (CDCl3): δ 2.32 (s, 4 H), 2.70 (s, 16 H). was bubbled NH3 (g) through a gas dispersion tube for 1 hour the white solid was filtered off washed with CHCl3 (4×100 mL) The combined filtrate was concentrated in vacuo to a white solid which was washed with diethyl ether (4×50 mL) dried under vacuum at ambient temperature A second crop of the free base was isolated from the ether to give a combined yield of 35.1 g (97.5%)