Hydrochloric Acid → HCID 69964135, compound

HRID 376541Notes

Reaction equation

HRID 376541 reaction equation
FC(F)(F)C(O)=O.[C:8]([C:11]1[CH:48]=[CH:47][C:14]([C:15]([NH:17][CH2:18][C:19]([N:21]2[CH2:26][CH2:25][N:24]([CH2:27][C:28]([OH:30])=[O:29])[C:23](=[O:31])[C@@H:22]2[CH2:32][CH2:33][CH2:34][NH:35][C:36](=[O:46])[C:37]2[CH:42]=[CH:41][C:40]([C:43](=[NH:45])[NH2:44])=[CH:39][CH:38]=2)=[O:20])=[O:16])=[CH:13][CH:12]=1)(=[NH:10])[NH2:9].[ClH:49]>>[ClH:49].[C:8]([C:11]1[CH:12]=[CH:13][C:14]([C:15]([NH:17][CH2:18][C:19]([N:21]2[CH2:26][CH2:25][N:24]([CH2:27][C:28]([OH:30])=[O:29])[C:23](=[O:31])[C@@H:22]2[CH2:32][CH2:33][CH2:34][NH:35][C:36](=[O:46])[C:37]2[CH:38]=[CH:39][C:40]([C:43](=[NH:44])[NH2:45])=[CH:41][CH:42]=2)=[O:20])=[O:16])=[CH:47][CH:48]=1)(=[NH:9])[NH2:10]

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 70307686HCID 70307686, compound

Product 1

HCID 69964135HCID 69964135, compound

Conditions

Temperature
0 °C

Procedure

In 5 ml of 0.5N hydrochloric acid was dissolved 1 g of (S)-4-(4-amidinobenzoylamino)acetyl-3-[3-(4-amidinobenzoylamino)propyl]-2-oxopiperazine-1-acetic acid trifluoroacetate produced in Working Example 2. The solution was stirred for 5 minutes at 0° C., which was allowed to be adsorbed on a CHP-20 column. The column was washed with water until the eluate showed neutral pH. The column was then subjected to elution with 10% acetonitrile/water. Fractions of the eluate were combined and freeze-dried to afford 0.7 g of the titled compound as a colorless amorphous powdery product.

Workup

  1. customproduced in Working Example 2
  2. washThe column was washed with water until the
  3. washThe column was then subjected to elution with 10% acetonitrile/water
  4. customfreeze-dried

Sources & evidence

ORD record
ord-e399bb8e253e458e9d44add5a3cd96b1
Source dataset
uspto-grants-2000_02
Patent number
US06020334

Reaction notes

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