1,2-Ethanedisulfonic Acid → 2-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid edisylate

HRID 582782

Reaktionsgleichung

Reaktionsgleichung von HRID 582782
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1[C:11]1[N:15]([C:16]2[CH:21]=[CH:20][C:19]([C:22](=[O:31])[N:23]([CH3:30])[CH2:24][CH2:25][CH2:26][N:27]([CH3:29])[CH3:28])=[CH:18][C:17]=2[CH:32]([CH3:34])[CH3:33])[N:14]=[C:13]([C:35]([NH:37][C:38]2([C:48]([OH:50])=[O:49])[CH:45]3[CH2:46][CH:41]4[CH2:42][CH:43]([CH2:47][CH:39]2[CH2:40]4)[CH2:44]3)=[O:36])[CH:12]=1.[CH2:51]([S:57]([OH:60])(=[O:59])=[O:58])[CH2:52][S:53]([OH:56])(=[O:55])=[O:54]>CC(O)C>[S:53]([CH2:52][CH2:51][S:57]([OH:60])(=[O:59])=[O:58])([OH:56])(=[O:55])=[O:54].[CH3:10][O:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[C:4]=1[C:11]1[N:15]([C:16]2[CH:21]=[CH:20][C:19]([C:22](=[O:31])[N:23]([CH3:30])[CH2:24][CH2:25][CH2:26][N:27]([CH3:28])[CH3:29])=[CH:18][C:17]=2[CH:32]([CH3:34])[CH3:33])[N:14]=[C:13]([C:35]([NH:37][C:38]2([C:48]([OH:50])=[O:49])[CH:39]3[CH2:40][CH:41]4[CH2:42][CH:43]([CH2:44][CH:45]2[CH2:46]4)[CH2:47]3)=[O:36])[CH:12]=1

Komponenten

4

Edukt 2

HCID 80321,2-Ethanedisulfonic AcidHCID 5311451SR142948A

Produkt 1

HCID 882310692-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid edisylateAusbeute 65,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

0.05 g of the compound obtained in EXAMPLE 1' and 0.04 g of the compound obtained in step A are dissolved in the heated state in 2 ml of 2-propanol, and the mixture is concentrated under vacuum. The residue is dissolved in 0.3 ml of water and 8 drops of dioxane, and crystallization is allowed to take place at RT. The crystallized product formed is drained, washed with water and dried at 90° C. under vacuum. 0.042 g of expected product is obtained, m.p.=266° C. (dec.).

Aufarbeitung

  1. concentrationthe mixture is concentrated under vacuum
  2. dissolutionThe residue is dissolved in 0.3 ml of water
  3. custom8 drops of dioxane, and crystallization
  4. customat RT
  5. customThe crystallized product formed
  6. washwashed with water
  7. customdried at 90° C. under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-684c97729c2b4e8aa267cbeeca152daa
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05925661

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