9-苄基-4-氧杂-1,9-二氮杂螺[5.5]十一烷-2-one

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

实验步骤: LAH (2.00 g, 52.7 mmol) was added to a THF (100 mL) solution containing 9-(phenylmethyl)-4-oxa-1,9-diazaspiro[5.5]undecan-2-one (3.1893 g, 12.3 mmol). The resulting mixture was stirred 1 h at reflux. The reaction was then cooled to room temperature and the following additions were made slowly: 2 mL of water followed by 2 mL of 1 N NaOH, and finally 4 mL of water. The mixture was then filtered and concentrated to give a thick clear oil (2.66 g, 88% yield). The material was used in the next step without further purification. LCMS-ESI (POS), M/Z, M+1. Found 247, Calculated 247. at reflux The mixture was then filtered concentrated

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Triethylamine (2 mL 14 mmol) was added to a DCM (50 mL) solution containing chloroacetyl chloride (1 mL, 14 mmol) and compound 391 (3 g, 14 mmol). The resulting mixture was stirred 2 h at 23° C. The solvent was stripped and THF was added followed by potassium tert-butoxide (5 g, 41 mmol). The resulting solution was stirred overnight at room temperature. The reaction was then concentrated to dryness and the resulting residue was washed with 200 mL of absolute ethanol. The ethanolic solution was then concentrated to give 3.16 g of 9-(phenylmethyl)-4-oxa-1,9-diazaspiro[5.5]undecan-2-one. The material was used in the next step without further purification. LCMS-ESI (POS), M/Z, M+1: Found 261, Calculated 261. The resulting solution was stirred overnight at room temperature The reaction was then concentrated to dryness the resulting residue was washed with 200 mL of absolute ethanol The ethanolic solution was then concentrated

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

实验步骤: LAH (2.00 g, 52.7 mmol) was added to a THF (100 mL) solution containing 9-(phenylmethyl)-4-oxa-1,9-diazaspiro[5.5]undecan-2-one (3.1893 g, 12.3 mmol). The resulting mixture was stirred 1 h at reflux. The reaction was then cooled to room temperature and the following additions were made slowly: 2 mL of water followed by 2 mL of 1 N NaOH, and finally 4 mL of water. The mixture was then filtered and concentrated to give a thick clear oil (2.66 g, 88% yield). The material was used in the next step without further purification. LCMS-ESI (POS), M/Z, M+1: Found 247, Calculated 247. at reflux The mixture was then filtered concentrated

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Triethylamine (2 mL 14 mmol) was added to a DCM (50 mL) solution containing chloroacetyl chloride (1 mL, 14 mmol) and compound 391 (3 g, 14 mmol). The resulting mixture was stirred 2 h at 23° C. The solvent was stripped and THF was added followed by potassium tert-butoxide (5 g, 41 mmol). The resulting solution was stirred overnight at room temperature. The reaction was then concentrated to dryness and the resulting residue was washed with 200 mL of absolute ethanol. The ethanolic solution was then concentrated to give 3.16 g of 9-(phenylmethyl)-4-oxa-1,9-diazaspiro[5.5]undecan-2-one. The material was used in the next step without further purification. LCMS-ESI (POS), M/Z, M+1: Found 261, Calculated 261. The resulting solution was stirred overnight at room temperature The reaction was then concentrated to dryness the resulting residue was washed with 200 mL of absolute ethanol The ethanolic solution was then concentrated

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

实验步骤: LAH (2.00 g, 52.7 mmol) was added to a THF (100 mL) solution containing 9-(phenylmethyl)-4-oxa-1,9-diazaspiro[5.5]undecan-2-one (3.1893 g, 12.3 mmol). The resulting mixture was stirred 1 h at reflux. The reaction was then cooled to room temperature and the following additions were made slowly: 2 mL of water followed by 2 mL of 1 N NaOH, and finally 4 mL of water. The mixture was then filtered and concentrated to give a thick clear oil (2.66 g, 88% yield). The material was used in the next step without further purification. LCMS-ESI (POS), M/Z, M+1. Found 247, Calculated 247. at reflux The mixture was then filtered concentrated

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Triethylamine (2 mL 14 mmol) was added to a DCM (50 mL) solution containing chloroacetyl chloride (1 mL, 14 mmol) and compound 391 (3 g, 14 mmol). The resulting mixture was stirred 2 h at 23° C. The solvent was stripped and THF was added followed by potassium tert-butoxide (5 g, 41 mmol). The resulting solution was stirred overnight at room temperature. The reaction was then concentrated to dryness and the resulting residue was washed with 200 mL of absolute ethanol. The ethanolic solution was then concentrated to give 3.16 g of 9-(phenylmethyl)-4-oxa-1,9-diazaspiro[5.5]undecan-2-one. The material was used in the next step without further purification. LCMS-ESI (POS), M/Z, M+1: Found 261, Calculated 261. The resulting solution was stirred overnight at room temperature The reaction was then concentrated to dryness the resulting residue was washed with 200 mL of absolute ethanol The ethanolic solution was then concentrated