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 2278837

反応式

HRID 2278837 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]>C1(C)C=CC=CC=1>[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

4

反応物 2

HCID 2132Ambroxol2 回HCID 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)

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

反応条件

温度
62.5 °C

実験手順

The mixture of ambroxol base (378.1 g, 1 mole) and toluene (3000 ml) was heated at 60-65° C. for 1-2 minutes to prepare a clear solution. Toluene (1900 ml) and theophylline-7-acetic acid (238.2 g, 1 mole) were charged in a round bottom flask and heated at 75 to 80° C. To this flask, the prepared solution of ambroxol base in toluene was added under stirring while maintaining the temperature between 75-80° C. during 2-3 minutes. The resulting reaction mixture was stirred at 100-105° C. for 25-30 minutes. The reaction mixture was allowed to cool to room temperature. The separated solid product was filtered and washed with toluene and dried. The yield of Acebrophylline obtained was 98%.

後処理

  1. customto prepare a clear solution
  2. temperatureheated at 75 to 80° C
  3. temperaturewhile maintaining the temperature between 75-80° C. during 2-3 minutes
  4. customThe resulting reaction mixture
  5. stirringwas stirred at 100-105° C. for 25-30 minutes
  6. temperatureto cool to room temperature
  7. filtrationThe separated solid product was filtered
  8. washwashed with toluene
  9. customdried

出典と根拠

ORDレコード
ord-df1417d907a34af5bb9b200241ea25f1
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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