Triethylamine → Lenalidomide

HRID 1843450ノート

反応式

HRID 1843450 の反応式
[CH2:1]1[CH:8]([N:9]2[C:13](=[O:14])[C:12]3[CH:15]=[CH:16][CH:17]=[C:18]([NH2:19])[C:11]=3[CH2:10]2)[C:6](=[O:7])[NH:5][C:3](=[O:4])[CH2:2]1.Cl.C(N(CC)CC)C>CO>[NH2:19][C:18]1[CH:17]=[CH:16][CH:15]=[C:12]2[C:11]=1[CH2:10][N:9]([CH:8]1[CH2:1][CH2:2][C:3](=[O:4])[NH:5][C:6]1=[O:7])[C:13]2=[O:14]

参加物

4

反応物 2

HCID 8471TriethylamineHCID 44234581Lenalidomide hydrochloride

生成物 1

HCID 216326Lenalidomide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
7.5 °C

実験手順

The lenalidomide hydrochloride salt was suspended in methanol (350 ml) and 1.1 mole equivalent of triethylamine was slowly added whilst stirring. The reaction mixture was stirred at ambient temperature for the next 45 minutes and then cooled at 5-10° C. and maintained at the same temperature for the next 45 minutes. The precipitated solid was filtered and dried. It was then washed with methanol (105 ml) and the resultant lenalidomide isolated by filtration. The pure product was dried at 50-55° C. and 150-200 mmHg pressure for about 7-8 hours.

後処理

  1. stirringThe reaction mixture was stirred at ambient temperature for the next 45 minutes
  2. temperaturemaintained at the same temperature for the next 45 minutes
  3. filtrationThe precipitated solid was filtered
  4. customdried
  5. washIt was then washed with methanol (105 ml)

出典と根拠

ORDレコード
ord-d30016703a354024900252e9ab2f34e8
出典データセット
uspto-grants-2015_02
特許番号
US08946265B2

反応ノート

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