7H-Pyrido[2,3-d]azepine-7-carboxylic acid, 2-amino-5,6,8,9-tetrahydro-, 1,1-dimethylethyl ester synthesis
- Product Name:7H-Pyrido[2,3-d]azepine-7-carboxylic acid, 2-amino-5,6,8,9-tetrahydro-, 1,1-dimethylethyl ester
- CAS Number:919099-35-7
- Molecular formula:C14H21N3O2
- Molecular Weight:263.34
![5H-Pyrido[2,3-d]azepin-2-amine, 6,7,8,9-tetrahydro-](/CAS/20210305/GIF/919099-34-6.gif)
Yield:919099-35-7 47%
Reaction Conditions:
Stage #1: 6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepin-2-ylaminewith potassium carbonate in dichloromethane at 20; for 0.166667 h;
Stage #2: di-tert-butyl dicarbonate in dichloromethane at 20; for 17 h;
Steps:
160.b
0.38 g (1.61 mmol) 6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepin-2-ylamine are suspended in 10 ml dichloromethane, then 0.667 g (4.83 mmol) potassium carbonate are added and the mixture is stirred at room temperature for 10 min. Then 0.369 g (1.69 mmol) BOC-anhydride in 10 ml dichloromethane is slowly added dropwise while cooling with ice, after which the mixture is stirred for 17 h at room temperature, diluted with 20 ml dichloromethane and washed with water. The crude product is dried with sodium sulphate, concentrated by evaporation and purified by chromatography through silica gel (eluant: dichloromethane/ethanol 98:2=>90:10).Yield: 0.20 g (47%)Rf value: 0.5 (silica gel; dichloromethane/ethanol=90:10)C14H21N3O2 (263.34)
References:
US2010/216769,2010,A1 Location in patent:Page/Page column 61
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