Hydrochloric Acid → Erlotinib hydrochloride

HRID 404533

反応式

HRID 404533 の反応式
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[C:10]2[C:12]([NH:16][C:17]3[CH:22]=[C:21]([C:23]#[CH:24])[CH:20]=[CH:19][CH:18]=3)=[N:13][CH:14]=[N:15][C:9]2=[CH:8][C:7]=1[O:25][CH2:26][CH2:27][O:28][CH3:29].[ClH:30]>CO>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[C:10]2[C:12]([NH:16][C:17]3[CH:18]=[CH:19][CH:20]=[C:21]([C:23]#[CH:24])[CH:22]=3)=[N:13][CH:14]=[N:15][C:9]2=[CH:8][C:7]=1[O:25][CH2:26][CH2:27][O:28][CH3:29].[ClH:30]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 176870Erlotinib2 回

生成物 1

HCID 176871Erlotinib hydrochloride収率 84.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
32.5 °C

実験手順

Into a 2 Lt. four necked round-bottomed flask provided with a mechanical stirrer, thermometer socket, reflux condenser etc., are charged 1340 mL of methanol, followed by Erlotinib base 60 g. (Prepared according to the process given in Example-(1) of PCT International Publication No. WO 2007/060691). The reaction mass is warmed to around 40° C. so that Erlotinib base completely dissolves. To this reaction mass, carbon treatment is given and the filtrate is transferred to another 2 Lt. four necked flask. To this solution isopropanolic HCl (HCl content as 100% is 6.12 g) is added in one lot and the reaction mass is stirred at 30-35° C. for about 90 minutes and filtered. The product is washed with fresh methanol and dried the wet cake to get 55.2 g of Erlotinib hydrochloride as a white crystalline powder.

後処理

  1. customfour necked round-bottomed flask provided with a mechanical stirrer
  2. temperaturethermometer socket, reflux condenser etc.
  3. custom(Prepared
  4. customThe reaction
  5. dissolutioncompletely dissolves
  6. filtrationfiltered
  7. washThe product is washed with fresh methanol
  8. customdried the wet cake

出典と根拠

ORDレコード
ord-9106fa1dbe6e4bf3b36718b48813247e
出典データセット
uspto-grants-2014_06
特許番号
US08748602B2

関連ノート

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