Acetic Anhydride → HCID 86686079, compound

HRID 400468Notes

Reaction equation

HRID 400468 reaction equation
CC(O[C:5]([CH3:7])=[O:6])=O.[F:8][C:9]([F:25])([F:24])[C:10]([N:12]1[CH2:18][CH2:17][C:16]2[CH:19]=[C:20]([NH2:23])[CH:21]=[CH:22][C:15]=2[CH2:14][CH2:13]1)=[O:11]>C(O)(=O)C.O>[F:25][C:9]([F:8])([F:24])[C:10]([N:12]1[CH2:18][CH2:17][C:16]2[CH:19]=[C:20]([NH:23][C:5](=[O:6])[CH3:7])[CH:21]=[CH:22][C:15]=2[CH2:14][CH2:13]1)=[O:11]

Participants

5

Procedure

2.75 mL acetanhydride was added to 5 g 3-trifluoracetyl-7-amino-1,2,4,5-tetrahydro-benzo[D]azepine in concentrated acetic acid. The mixture was stirred 17 h at RT, diluted with water and stirred for another 1 h at RT. The precipitate was filtered, washed with water and dried to give 5.35 g of the desired product. Rf: 0.46 (DCM/MeOH=19/1), (M+H)+=301

Workup

  1. stirringstirred for another 1 h at RT
  2. filtrationThe precipitate was filtered
  3. washwashed with water
  4. customdried

Sources & evidence

ORD record
ord-77a892ae55134e77b9c7887eb7cd49f9
Source dataset
uspto-grants-2014_06
Patent number
US08741892B2

Reaction notes

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