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

反応式

HRID 582782 の反応式
[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

参加物

4

反応物 2

HCID 80321,2-Ethanedisulfonic AcidHCID 5311451SR142948A

生成物 1

HCID 882310692-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid edisylate収率 65.8%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-684c97729c2b4e8aa267cbeeca152daa
出典データセット
uspto-grants-1999_07
特許番号
US05925661

関連ノート

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