Methanesulfonic Acid → Erlotinib Hydrochloride

HRID 238995

反応式

HRID 238995 の反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:17][CH2:18][CH2:19][O:20][CH3:21])=[C:9]([O:12][CH2:13][CH2:14][O:15][CH3:16])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[NH2:22][C:23]1[CH:24]=[C:25]([C:29]#[CH:30])[CH:26]=[CH:27][CH:28]=1.CS(O)(=O)=O>>[CH3:16][O:15][CH2:14][CH2:13][O:12][C:9]1[CH:10]=[C:11]2[C:2]([NH:22][C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([C:29]#[CH:30])[CH:24]=3)=[N:3][CH:4]=[N:5][C:6]2=[CH:7][C:8]=1[O:17][CH2:18][CH2:19][O:20][CH3:21].[ClH:1]

参加物

4

反応物 3

HCID 6395Methanesulfonic AcidHCID 104682Benzenamine, 3-ethynyl-HCID 112899424-Chloro-6,7-bis(2-methoxyethoxy)quinazoline

生成物 1

HCID 176871Erlotinib Hydrochloride

反応条件

温度
27.5 °C

実験手順

5 g of 4-chloro-6,7-bis(2-methoxyethoxy) quinazoline was suspended in 150 ml denatured spirit (SPDS) and 4.6 g of 3-aminophenyl acetylene was charged at 25-30° C. Further 1.0 ml of methane sulphonic acid was added. The reaction mass was stirred at 25-30° C. for 3 hours. Solid obtained was filtered, washed with SPDS and dried under vacuum. This solid was suspended in water, basified with ammonia and stirred for 10 minutes. The resulting erlotinib base was isolated, washed with water and dried under vacuum. The base was suspended in water and acidified to pH 1.0-2.0 using hydrochloric acid. The reaction mixture was stirred for 2 hours, filtered, washed with water and dried at 40-45° C. to obtain 5.8 g of erlotinib hydrochloride.

後処理

  1. additionwas charged at 25-30° C
  2. customSolid obtained
  3. filtrationwas filtered
  4. washwashed with SPDS
  5. customdried under vacuum
  6. stirringstirred for 10 minutes

出典と根拠

ORDレコード
ord-84b9bfb18bbe48c0987fa54d56495d84
出典データセット
uspto-grants-2014_02
特許番号
US08642758B2

関連ノート

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