Methanol → Erlotinib

HRID 523964

反応式

HRID 523964 の反応式
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:20]([NH:21][C:22]3[CH:23]=[CH:24][CH:25]=[C:26]([C:28]#[CH:29])[CH:27]=3)=[N:19][CH:18]=[N:17][C:9]2=[CH:10][C:11]=1[O:12][CH2:13][CH2:14][O:15][CH3:16].Cl.CO.C(=O)([O-])[O-].[Na+].[Na+]>O>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:20]([NH:21][C:22]3[CH:27]=[C:26]([C:28]#[CH:29])[CH:25]=[CH:24][CH:23]=3)=[N:19][CH:18]=[N:17][C:9]2=[CH:10][C:11]=1[O:12][CH2:13][CH2:14][O:15][CH3:16]

参加物

5

反応物 3

HCID 887MethanolHCID 10340Sodium CarbonateHCID 176871Erlotinib hydrochloride

生成物 1

HCID 176870Erlotinib

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
27.5 °C

実験手順

The wet cake of crude erlotinib hydrochloride was added to 500 ml (10 vol.) of methanol under stirring at 25-30° C. to obtain a suspension. Sodium carbonate (33.8 g, 0.3197 mol) was added to the mixture at 25-30° C. and stirred for one hour at 25-30° C. 500 ml (10 vol.) of water was added to the reaction mixture and stirred for one hour. The crude erlotinib base was isolated by filtration and suck dried before adding it to 250 ml (5 vol.) of water at 25-30° C. and stirred for 30 min. The erlotinib base was isolated by filtration and washed with 50 ml (1 vol.) of water and suck dried to get 70 g as a wet cake. This wet cake was dried under reduced pressure at 100 mm Hg for 3 hour at 60-65° C. to afford 63 g of erlotinib base as an off-white powder.

後処理

  1. customto obtain a suspension
  2. stirringstirred for one hour at 25-30° C
  3. stirringstirred for one hour
  4. customThe crude erlotinib base was isolated by filtration and suck
  5. customdried
  6. additionbefore adding it to 250 ml (5 vol.) of water at 25-30° C.
  7. stirringstirred for 30 min

出典と根拠

ORDレコード
ord-7429b4506f93491b95fa1bc5f76707f9
出典データセット
uspto-grants-2016_05
特許番号
US09340515B2

関連ノート

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