Ambroxol → (1,3-Dimethyl-2,6-dioxo-1,2,3,6-tetrahydro-7H-purin-7-yl)acetic acid--4-(((2-amino-3,5-dibromophenyl)methyl)amino)cyclohexan-1-ol (1/1)

HRID 2278833

反応式

HRID 2278833 の反応式
[CH2:1]1[CH:6]([NH:7][CH2:8][C:9]2[C:14]([NH2:15])=[C:13]([Br:16])[CH:12]=[C:11]([Br:17])[CH:10]=2)[CH2:5][CH2:4][CH:3]([OH:18])[CH2:2]1.[N:19]1([C:30](=[O:31])[C:29]2[N:28]([CH2:32][C:33]([OH:35])=[O:34])[CH:27]=[N:26][C:25]=2[N:23]([CH3:24])[C:21]1=[O:22])[CH3:20]>>[CH3:24][N:23]1[C:21](=[O:22])[N:19]([CH3:20])[C:30](=[O:31])[C:29]2[N:28]([CH2:32][C:33]([OH:35])=[O:34])[CH:27]=[N:26][C:25]1=2.[CH2:5]1[CH:6]([NH:7][CH2:8][C:9]2[C:14]([NH2:15])=[C:13]([Br:16])[CH:12]=[C:11]([Br:17])[CH:10]=2)[CH2:1][CH2:2][CH:3]([OH:18])[CH2:4]1

参加物

3

反応物 2

HCID 2132AmbroxolHCID 69550Acefylline

生成物 1

HCID 176595(1,3-Dimethyl-2,6-dioxo-1,2,3,6-tetrahydro-7H-purin-7-yl)acetic acid--4-(((2-amino-3,5-dibromophenyl)methyl)amino)cyclohexan-1-ol (1/1)

反応条件

温度
72.5 °C

実験手順

The solution of ambroxol base in non-polar solvent is added to the flask containing theophylline-7-acetic acid and non-polar solvent under stirring while maintaining the temperature between 60-85° C. The addition time is 2-3 minutes. The reaction mixture is heated at the temperature between 60-105° C. with continuous stirring for 25-35 minutes. The reaction mixture is allowed to cool to the room temperature. A solid product is formed. This solid product is separated by filtration. The product is washed with the small amount of non-polar solvent and dried. The yield of Acebrophylline obtained is 95-98% of the theoretical yield. The yield of Acebrophylline is 154-159% of the weight of ambroxol base. The purity of Acebrophylline thus obtained as measured by HPLC is more than 99%.

後処理

  1. temperatureThe reaction mixture is heated at the temperature between 60-105° C.
  2. stirringwith continuous stirring for 25-35 minutes
  3. temperatureto cool to the room temperature
  4. customA solid product is formed
  5. customThis solid product is separated by filtration
  6. washThe product is washed with the small amount of non-polar solvent
  7. customdried

出典と根拠

ORDレコード
ord-f4ce023b849e4fb5b5ef86fa0c3a6670
出典データセット
uspto-grants-2015_09
特許番号
US09133196B2

関連ノート

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