Sodium Azide → HCID 22902051, compound

HRID 1489554Notes

Reaction equation

Cl[CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:12][C:5]=2[NH:4][C:3]1=[O:19].[N-:20]=[N+:21]=[N-:22].[Na+]>CS(C)=O>[N:20]([CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:12][C:5]=2[NH:4][C:3]1=[O:19])=[N+:21]=[N-:22]

Participants

Conditions

Temperature: 80 °C

Procedure

A mixture comprising 0.93 g (3.42 mmol) of 3-chloro-8-phenyl-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one obtained in the Synthesis Example A-5, 0.27 g (4.18 mmol) of sodium azide and 15 ml of dimethyl sulfoxide was stirred at 80° C. for 3 hours. After further adding 0.05 g of sodium azide and stirring for 30 minutes, the reaction mixture was added to ice water. The crystals were collected by filtration and dried under reduced pressure to thereby give 0.77 g of the title compound. Yield 81%.

Workup

stirringstirring for 30 minutes
filtrationThe crystals were collected by filtration
customdried under reduced pressure

Sources & evidence

ORD record: ord-0e3c9c4ac4714b1db8ec4993ac3e72e5
Source dataset: uspto-grants-1997_10
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05679671

Reaction notes

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