Hydrochloric Acid → HCID 19081311, compound

HRID 963487Notes

Reaction equation

HRID 963487 reaction equation
C(OC([NH:8][CH:9]1[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[F:22])[C:13]2[CH:23]=[CH:24][CH:25]=[CH:26][C:12]=2[N:11]([CH2:27][C:28]2[C:33]([C:34]([O:36][CH3:37])=[O:35])=[CH:32][CH:31]=[CH:30][N:29]=2)[C:10]1=[O:38])=O)(C)(C)C.Cl>C(Cl)(Cl)Cl>[NH2:8][CH:9]1[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[F:22])[C:13]2[CH:23]=[CH:24][CH:25]=[CH:26][C:12]=2[N:11]([CH2:27][C:28]2[C:33]([C:34]([O:36][CH3:37])=[O:35])=[CH:32][CH:31]=[CH:30][N:29]=2)[C:10]1=[O:38]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 67687966HCID 67687966, compound

Product 1

HCID 19081311HCID 19081311, compoundYield 99.1%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A solution of (3RS)-3-tert-butoxycarbonylamino-2,3-dihydro-5-(2-fluorophenyl)-1-(3-methoxycarbonylpyridin-2-yl) methyl-1H-1,4-benzodiazepin-2-one (0.80 g) in chloroform (10 ml) was treated with hydrogen chloride at room temperature and the mixture was stirred for 1 hour under the same condition. The mixture was concentrated in vacuo and the residue was taken up with chloroform. The organic layer was washed with a saturated sodium carbonate aqueous solution, dried over sodium sulfate, filtered and concentrated in vacuo to give (3RS)-3-amino-2,3-dihydro-5-(2-fluorophenyl)-1-(3-methoxycarbonylpyridin-2-yl)methyl-1H-1,4-benzodiazepin-2-one (0.64 g) as a colorless form.

Workup

  1. concentrationThe mixture was concentrated in vacuo
  2. washThe organic layer was washed with a saturated sodium carbonate aqueous solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-bf971e3af820473abe66369e81eeee80
Source dataset
uspto-grants-1998_06
Patent number
US05763437

Reaction notes

Loading…