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Trifluoroacetic acid → HCID 70303465, compound

HRID 376540
Notes
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Reaction equation

HRID 376540 reaction equation
[C:1]([C:4]1[CH:40]=[CH:39][C:7]([C:8]([NH:10][CH2:11][CH2:12][CH2:13][C@@H:14]2[N:19]([C:20](=[O:33])[CH2:21][NH:22][C:23](OCC3C=CC=CC=3)=[O:24])[CH2:18][CH2:17][N:16]([CH2:34][C:35]([OH:37])=[O:36])[C:15]2=[O:38])=[O:9])=[CH:6][CH:5]=1)(=[NH:3])[NH2:2].ON1C(=O)CCC1=O.C(OC([NH:56][CH2:57][CH2:58][C:59]1[CH:67]=[CH:66][C:62](C(O)=O)=[CH:61][CH:60]=1)=O)(C)(C)C.Cl.C(N=C=NCCCN(C)C)C.[F:80][C:81]([F:86])([F:85])[C:82]([OH:84])=[O:83]>CO.[H][H].CN(C)C=O>[F:80][C:81]([F:86])([F:85])[C:82]([OH:84])=[O:83].[NH2:56][CH2:57][CH2:58][C:59]1[CH:67]=[CH:66][C:62]([C:23]([NH:22][CH2:21][C:20]([N:19]2[CH2:18][CH2:17][N:16]([CH2:34][C:35]([OH:37])=[O:36])[C:15](=[O:38])[C@@H:14]2[CH2:13][CH2:12][CH2:11][NH:10][C:8](=[O:9])[C:7]2[CH:39]=[CH:40][C:4]([C:1](=[NH:3])[NH2:2])=[CH:5][CH:6]=2)=[O:33])=[O:24])=[CH:61][CH:60]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 5

HCID 6422Trifluoroacetic acidHCID 80170N-HydroxysuccinimideHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 11103621HCID 11103621, compoundHCID 166409054-(2-{[(Tert-butoxy)carbonyl]amino}ethyl)benzoic acid

Product 1

HCID 70303465
HCID 70303465, compound

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 6228DimethylformamideSolvent2×HCID 178418361HCID 178418361, compoundSolvent

Procedure

In 20 ml of methanol was dissolved 300 mg of (S)-3-[3-(4-amidinobenzoylamino)propyl]-4-benzyloxycarbonylaminoacetyl-2-oxopiperazine-1-acetic acid produced in Reference Example 21. To the solution was added 120 mg of 10% Pd--C, and the mixture was stirred for one hour at room temperature in hydrogen streams. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure to give an oily product, which was dissolved in 5 ml of dimethylformamide. To the solution was added 5 ml of activated-ester solution in dimethylformamide which was prepared from 94 mg of N-hydroxysuccinimide and 173 mg of 4-(2-t-butoxycarbonylaminoethyl)benzoic acid in the presence of 167 mg of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride. The mixture was stirred for two hours at room temperature. The reaction mixture was concentrated to give an oily product, which was dissolved in 7 ml of trifluoroacetic acid. The solution was stirred for one hour at room temperature. The reaction mixture was concentrated under reduced pressure to give a crude product, which was purified by means of a CHP-20 column (eluted with 10% acetonitrile/water) to afford 110 mg of the titled compound as a colorless amorphous powdery product.

Workup

  1. customproduced in Reference Example 21
  2. filtrationThe catalyst was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customto give an oily product, which
  5. concentrationThe reaction mixture was concentrated
  6. customto give an oily product, which
  7. stirringThe solution was stirred for one hour at room temperature
  8. concentrationThe reaction mixture was concentrated under reduced pressure
  9. customto give a crude product, which
  10. customwas purified by means of a CHP-20 column (eluted with 10% acetonitrile/water)

Sources & evidence

ORD record
ord-82287e66446746148c8ede166f4f9905
Source dataset
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06020334

Reaction notes

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