反応 #4132938
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-f5fcda6afb844215bedc6367e9bef717表示可能な構造データがありません
C(C(Cl)(Cl)Cl)(OC(=O)Cl)Cl製品情報
1,2,2,2-tetrachloroethyl carbonochloridate (CAS 98015-53-3) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 2733327
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
12 反応 · 12 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-f5fcda6afb844215bedc6367e9bef717反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-f5fcda6afb844215bedc6367e9bef717反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-f5fcda6afb844215bedc6367e9bef717反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of astaxanthin 2E (0.100 g, 0.168 mmol) in DCM (4 mL) at 0° C. was added DIPEA (0.585 mL, 3.36 mmol), and 1,2,2,2-tetrachloroethyl chloroformate (0.103 mL, 0.672 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature for 1.5 hours, at which time (D)-mannitol (0.3060 g, 1.68 mmol), DMF (3 mL), and DMAP (0.2052 g, 1.68 mmol) were added to the reaction. The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction was diluted with DCM, quenched with brine (20 mL), and then extracted with DCM. The combined organic layers were concentrated to yield mannitol monocarbonate (LVII) (10.19%) HPLC retention time: 9.474 min., 10.19% (AUC); LRMS (ESI) m/z (relative intensity): 827 (M++Na) (50), 804 (M+) (25), 725 (58), 613 (100), and astaxanthin 2E (53.73%). at room temperature for 1.5 hours The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction quenched with brine (20 mL) extracted with DCM The combined organic layers were concentrated
ソース ID: ord-1d0f8210da6d4ad386a59e203537d222反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of astaxanthin 2E (0.100 g, 0.168 mmol) in DCM (4 mL) at 0° C. was added DIPEA (0.585 mL, 3.36 mmol), and 1,2,2,2-tetrachloroethyl chloroformate (0.103 mL, 0.672 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature for 1.5 hours, at which time (D)-mannitol (0.3060 g, 1.68 mmol), DMF (3 mL), and DMAP (0.2052 g, 1.68 mmol) were added to the reaction. The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction was diluted with DCM, quenched with brine (20 mL), and then extracted with DCM. The combined organic layers were concentrated to yield mannitol monocarbonate (LVII) (10.19%) HPLC retention time: 9.474 min., 10.19% (AUC); LRMS (ESI) m/z (relative intensity): 827 (M++Na) (50), 804 (M+) (25), 725 (58), 613 (100), and astaxanthin (53.73%). at room temperature for 1.5 hours The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction quenched with brine (20 mL) extracted with DCM The combined organic layers were concentrated
ソース ID: ord-a32bfa06c6ea47a3afd9db4fcef6b0b9反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of astaxanthin 2E (0.100 g, 0.168 mmol) in DCM (4 mL) at 0° C. was added DIPEA (0.585 mL, 3.36 mmol), and 1,2,2,2-tetrachloroethyl chloroformate (0.103 mL, 0.672 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature for 1.5 hours, at which time (D)-mannitol (0.3060 g, 1.68 mmol), DMF (3 mL), and DMAP (0.2052 g, 1.68 mmol) were added to the reaction. The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction was diluted with DCM, quenched with brine (20 mL), and then extracted with DCM. The combined organic layers were concentrated to yield mannitol monocarbonate (LVII) (10.19%) HPLC retention time: 9.474 min., 10.19% (AUC); LRMS (ESI) m/z (relative intensity): 827 (M++Na) (50), 804 (M+) (25), 725 (58), 613 (100), and astaxanthin (53.73%). at room temperature for 1.5 hours The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction quenched with brine (20 mL) extracted with DCM The combined organic layers were concentrated
ソース ID: ord-a32bfa06c6ea47a3afd9db4fcef6b0b9反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 34.7 ml (0.4 mmol) of methylamine (in 40% strength aqueous solution) are added dropwise to a solution maintained at 0° C. of 49.4 g (0.2 mole) of 1,2,2,2-tetrachloroethyl chloroformate in dichloromethane (150 ml). The mixture is then stirred for 2 hours at room temperature. The organic phase is washed with 2×100 ml of water and dried over magnesium sulphate. The organic phase is washed with 2×100 ml of water dried over magnesium sulphate
ソース ID: ord-15c439ed99fb49c6bfd27dedef4a3286反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 34.7 ml (0.4 mmol) of methylamine (in 40% strength aqueous solution) are added dropwise to a solution maintained at 0° C. of 49.4 g (0.2 mole) of 1,2,2,2-tetrachloroethyl chloroformate in dichloromethane (150 ml). The mixture is then stirred for 2 hours at room temperature. The organic phase is washed with 2×100 ml of water and dried over magnesium sulphate. The organic phase is washed with 2×100 ml of water dried over magnesium sulphate
ソース ID: ord-15c439ed99fb49c6bfd27dedef4a3286反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of astaxanthin 2E (0.100 g, 0.168 mmol) in DCM (4 mL) at 0° C. was added DIPEA (0.585 mL, 3.36 mmol), and 1,2,2,2-tetrachloroethyl chloroformate (0.103 mL, 0.672 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature for 1.5 hours, at which time (D)-mannitol (0.3060 g, 1.68 mmol), DMF (3 mL), and DMAP (0.2052 g, 1.68 mmol) were added to the reaction. The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction was diluted with DCM, quenched with brine (20 mL), and then extracted with DCM. The combined organic layers were concentrated to yield mannitol monocarbonate (LVII) (10.19%) HPLC retention time: 9.474 min., 10.19% (AUC); LRMS (ESI) m/z (relative intensity): 827 (M++Na) (50), 804 (M+) (25), 725 (58), 613 (100), and astaxanthin 2E (53.73%). at room temperature for 1.5 hours The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction quenched with brine (20 mL) extracted with DCM The combined organic layers were concentrated
ソース ID: ord-d4890103dc8747b896b953c38170efaa反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of astaxanthin 2E (0.100 g, 0.168 mmol) in DCM (4 mL) at 0° C. was added DIPEA (0.585 mL, 3.36 mmol), and 1,2,2,2-tetrachloroethyl chloroformate (0.103 mL, 0.672 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature for 1.5 hours, at which time (D)-mannitol (0.3060 g, 1.68 mmol), DMF (3 mL), and DMAP (0.2052 g, 1.68 mmol) were added to the reaction. The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction was diluted with DCM, quenched with brine (20 mL), and then extracted with DCM. The combined organic layers were concentrated to yield mannitol monocarbonate (LVII) (10.19%) HPLC retention time: 9.474 min., 10.19% (AUC); LRMS (ESI) m/z (relative intensity): 827 (M++Na) (50), 804 (M+) (25), 725 (58), 613 (100), and as (53.73%). at room temperature for 1.5 hours The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction quenched with brine (20 mL) extracted with DCM The combined organic layers were concentrated
ソース ID: ord-3cda3aee046742a5920a2394d3eda78f反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of astaxanthin 2E (0.100 g, 0.168 mmol) in DCM (4 mL) at 0° C. was added DIPEA (0.585 mL, 3.36 mmol), and 1,2,2,2-tetrachloroethyl chloroformate (0.103 mL, 0.672 mmol). The reaction mixture was stirred at 0° C. for 2 hours, then at room temperature for 1.5 hours, at which time (D)-mannitol (0.3060 g, 1.68 mmol), DMF (3 mL), and DMAP (0.2052 g, 1.68 mmol) were added to the reaction. The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction was diluted with DCM, quenched with brine (20 mL), and then extracted with DCM. The combined organic layers were concentrated to yield mannitol monocarbonate (LVII) (10.19%) HPLC retention time: 9.474 min., 10.19% (AUC); LRMS (ESI) m/z (relative intensity): 827 (M++Na) (50), 804 (M+) (25), 725 (58), 613 (100), and as (53.73%). at room temperature for 1.5 hours The reaction mixture was stirred at room temperature for 24 hours, at which time the reaction quenched with brine (20 mL) extracted with DCM The combined organic layers were concentrated
ソース ID: ord-3cda3aee046742a5920a2394d3eda78f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 34.7 ml (0.4 mmol) of methylamine (in 40% strength aqueous solution) are added dropwise to a solution maintained at 0° C. of 49.4 g (0.2 mole) of 1,2,2,2-tetrachloroethyl chloroformate in dichloromethane (150 ml). The mixture is then stirred for 2 hours at room temperature. The organic phase is washed with 2×100 ml of water and dried over magnesium sulphate. The organic phase is washed with 2×100 ml of water dried over magnesium sulphate
ソース ID: ord-15c439ed99fb49c6bfd27dedef4a3286PubChem References
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