Sorafenib → Sorafenib Tosylate

HRID 332935

반응식

HRID 332935 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:28]=[CH:27][C:15]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]([C:23]([NH:25][CH3:26])=[O:24])[CH:18]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][C:3]=1[C:29]([F:32])([F:31])[F:30].O.[C:34]1([CH3:44])[CH:39]=[CH:38][C:37]([S:40]([OH:43])(=[O:42])=[O:41])=[CH:36][CH:35]=1>C(O)C>[S:40]([C:37]1[CH:38]=[CH:39][C:34]([CH3:44])=[CH:35][CH:36]=1)([OH:43])(=[O:42])=[O:41].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:28]=[CH:27][C:15]([O:16][C:17]3[CH:22]=[CH:21][N:20]=[C:19]([C:23]([NH:25][CH3:26])=[O:24])[CH:18]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][C:3]=1[C:29]([F:32])([F:30])[F:31]

참가 물질

4

반응물 2

HCID 216239SorafenibHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 406563Sorafenib Tosylate수율 91.3%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

903 g of 4-{4-[({[4-chloro-3-(trifluoromethyl)phenyl]amino}carbonyl)amino]phenoxy}-N-methyl-pyridine-2-carboxamide, prepared as described in WO 00/42012, are initially charged in 2700 ml of ethanol. 451.7 g of p-toluenesulfonic acid monohydrate are dissolved in 1340 g of ethanol and added dropwise at room temperature. The suspension is stirred at room temperature for 1 hour, then filtered off with suction, and the residue is washed three times with 830 ml each time of ethanol. The drying is effected at 50° C. under reduced pressure with supply of air. 1129.6 g of the title compound in the polymorph II are obtained.

후처리

  1. additionadded dropwise at room temperature
  2. filtrationfiltered off with suction
  3. washthe residue is washed three times with 830 ml each time of ethanol
  4. customis effected at 50° C. under reduced pressure

출처 및 근거

ORD 기록
ord-c968c0b3de584495a5d0a7769e6e977e
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877933B2

연결된 노트

불러오는 중…