Methanol → Erlotinib

HRID 523964

반응식

HRID 523964 반응식
[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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 10340Sodium CarbonateHCID 176871Erlotinib hydrochloride

생성물 1

HCID 176870Erlotinib

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
27.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7429b4506f93491b95fa1bc5f76707f9
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340515B2

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