2,2-dimethyl-3,4-dihydro-1,4-benzoxazepin-5-one

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: After adding phosphorous oxychloride (5 mL) and phosphorous pentachloride (0.65 g, 3.13 mmol) to 2,2-dimethyl-3,4-dihydro-2H-benzo[f][1,4]oxazepin-5-one (0.60 g, 3.13 mmol) (refer to the aforementioned Non-Patent Document 3 for a description of the synthesis method) at room temperature, the mixture was refluxed while heating for 5.5 hours. After allowing to cool to room temperature, the mixture was concentrated under reduced pressure and the residue was poured over crushed ice. The aqueous layer was extracted with ethyl acetate (50 mL) and the combined organic layer was washed twice with “saturated aqueous sodium bicarbonate solution (30 mL)+H2O (20 mL) and then with brine (30 mL) followed by drying with magnesium sulfate. After filtering, the solvent was distilled off under reduced pressure to obtain 0.74 g of 5-chloro-2,2-dimethyl-2,3-dihydro-benzo[f][1,4]oxazepine in the form of a brown oily substance. This substance was used in the next reaction without purifying further. refer to the aforementioned Non-Patent Document 3 for a description of the synthesis method) at room temperature the mixture was refluxed while heating for 5.5 hours the mixture was concentrated under reduced pressure the residue was poured over crushed ice The aqueous layer was extracted with ethyl acetate (50 mL) the combined organic layer was washed twice with “saturated aqueous sodium bicarbonate solution (30 mL)+H2O (20 mL) by drying with magnesium sulfate After filtering the solvent was distilled off under reduced pressure

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: After adding phosphorous oxychloride (5 mL) and phosphorous pentachloride (0.65 g, 3.13 mmol) to 2,2-dimethyl-3,4-dihydro-2H-benzo[f][1,4]oxazepin-5-one (0.60 g, 3.13 mmol) (refer to the aforementioned Non-Patent Document 3 for a description of the synthesis method) at room temperature, the mixture was refluxed while heating for 5.5 hours. After allowing to cool to room temperature, the mixture was concentrated under reduced pressure and the residue was poured over crushed ice. The aqueous layer was extracted with ethyl acetate (50 mL) and the combined organic layer was washed twice with “saturated aqueous sodium bicarbonate solution (30 mL)+H2O (20 mL) and then with brine (30 mL) followed by drying with magnesium sulfate. After filtering, the solvent was distilled off under reduced pressure to obtain 0.74 g of 5-chloro-2,2-dimethyl-2,3-dihydro-benzo[f][1,4]oxazepine in the form of a brown oily substance. This substance was used in the next reaction without purifying further. refer to the aforementioned Non-Patent Document 3 for a description of the synthesis method) at room temperature the mixture was refluxed while heating for 5.5 hours the mixture was concentrated under reduced pressure the residue was poured over crushed ice The aqueous layer was extracted with ethyl acetate (50 mL) the combined organic layer was washed twice with “saturated aqueous sodium bicarbonate solution (30 mL)+H2O (20 mL) by drying with magnesium sulfate After filtering the solvent was distilled off under reduced pressure