HCID 9846037, compound → HCID 70292997, compound

HRID 1417230Notes

Reaction equation

HRID 1417230 reaction equation
[C:1]([C:4]1[CH:32]=[CH:31][C:7]([O:8][CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][N:15]([CH:18]([C:23]3[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=3)[CH2:19][C:20]([OH:22])=[O:21])[C:14](=[O:29])[C:13]2=[O:30])=[CH:6][CH:5]=1)(=[NH:3])[NH2:2]>O>[OH2:8].[OH2:8].[OH2:8].[C:1]([C:4]1[CH:5]=[CH:6][C:7]([O:8][CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][N:15]([CH:18]([C:23]3[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=3)[CH2:19][C:20]([OH:22])=[O:21])[C:14](=[O:29])[C:13]2=[O:30])=[CH:31][CH:32]=1)(=[NH:2])[NH2:3]

Participants

3

Reactant 1

HCID 9846037HCID 9846037, compound

Product 1

HCID 70292997HCID 70292997, compoundYield 296.4%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

In 20 ml of water was suspended 3.1 g of the (-)-3-[4-[3-(4-amidinophenoxy)propyl]-2,3-dioxopiperazin-1-yl]-3-(pyridin-3-yl)propionic acid obtained in Example 57, and the suspension was heated to obtain a homogeneous solution. This solution was allowed to stand overnight at room temperature, after which the crystals precipitated were collected by filtration, washed with 3 ml of water, and then dried at room temperature to obtain 2.58 g of (-)-3-[4-[3-(4-amidinophenoxy) propyl]-2,3-dioxopiperazin-1-yl]-3-(pyridin-3-yl) propionic acid trihydrate as colorless crystals having a melting point of 238°-240° C. (decomp.).

Workup

  1. temperaturethe suspension was heated
  2. customto obtain a homogeneous solution
  3. customafter which the crystals precipitated
  4. filtrationwere collected by filtration
  5. washwashed with 3 ml of water
  6. customdried at room temperature

Sources & evidence

ORD record
ord-b2bd8aeaf86f433dbd2126a63ecb848f
Source dataset
uspto-grants-1999_03
Patent number
US05877174

Reaction notes

Loading…