Hydrochloric Acid → Erlotinib hydrochloride

HRID 404533

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HRID 404533 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 176870Erlotinib2회

생성물 1

HCID 176871Erlotinib hydrochloride수율 84.2%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
32.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9106fa1dbe6e4bf3b36718b48813247e
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748602B2

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