Trifluoroacetic acid → HCID 178510102, compound

HRID 268135Notes

Reaction equation

HRID 268135 reaction equation
FC(F)(F)C(O)=O.C(OC([NH:15][CH2:16][C:17]1[CH2:22][CH2:21][CH2:20][CH2:19][C:18]=1[CH2:23][C:24]([NH:26][CH:27]1[C:44](=[O:45])[N:29]2[C:30]([C:41]([OH:43])=[O:42])=[C:31]([CH2:34][S:35][C:36]3[N:37]=[N:38][NH:39][CH:40]=3)[CH2:32][S:33][C@H:28]12)=[O:25])=O)(C)(C)C>CCOCC>[NH2:15][CH2:16][C:17]1[CH2:22][CH2:21][CH2:20][CH2:19][C:18]=1[CH2:23][C:24]([NH:26][CH:27]1[C:44](=[O:45])[N:29]2[C:30]([C:41]([OH:43])=[O:42])=[C:31]([CH2:34][S:35][C:36]3[N:37]=[N:38][NH:39][CH:40]=3)[CH2:32][S:33][C@H:28]12)=[O:25]

Participants

4

Procedure

A mixture of trifluoroacetic acid (1 ml.) and 5h (0.55 g., 0.98 mmoles) was stirred for 30 min. at room temperature and diluted with ether (50 ml.) to give the precipitate which was collected by filtration and slurried in a small amount of water (2 ml.). The mixture was adjusted to pH 6 with ammonium hydroxide and diluted with acetonitrile (200 ml.) to precipitate 6h which was washed with acetonitrile (50 ml.). Yield 0.36 g. (80%). M.p. 203° - 215° C. (dec.).

Workup

  1. customto give the precipitate which
  2. filtrationwas collected by filtration
  3. additiondiluted with acetonitrile (200 ml.)
  4. customto precipitate 6h which
  5. washwas washed with acetonitrile (50 ml.)

Sources & evidence

ORD record
ord-1b535539a7b2473288ce956dac33f3bb
Source dataset
uspto-grants-1976_03
Patent number
US03946000

Reaction notes

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