Benzenesulfonic Acid → 4{4-[3-(4-Chloro-3-trifluoromethylphenyl)-ureido]-3-fluorophenoxy}-pyridine-2-carboxylic acid methylamide phenylsulfonate

HRID 475443노트

반응식

HRID 475443 반응식
[CH3:1][NH:2][C:3]([C:5]1[CH:10]=[C:9]([O:11][C:12]2[CH:17]=[CH:16][C:15]([NH:18][C:19]([NH:21][C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([C:29]([F:32])([F:31])[F:30])[CH:23]=3)=[O:20])=[C:14]([F:33])[CH:13]=2)[CH:8]=[CH:7][N:6]=1)=[O:4].[C:34]1([S:40]([OH:43])(=[O:42])=[O:41])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>C(O)C>[C:34]1([S:40]([OH:43])(=[O:42])=[O:41])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.[CH3:1][NH:2][C:3]([C:5]1[CH:10]=[C:9]([O:11][C:12]2[CH:17]=[CH:16][C:15]([NH:18][C:19]([NH:21][C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([C:29]([F:32])([F:31])[F:30])[CH:23]=3)=[O:20])=[C:14]([F:33])[CH:13]=2)[CH:8]=[CH:7][N:6]=1)=[O:4]

참가 물질

4

반응물 2

HCID 7371Benzenesulfonic AcidHCID 11167602Regorafenib

생성물 1

HCID 874054824{4-[3-(4-Chloro-3-trifluoromethylphenyl)-ureido]-3-fluorophenoxy}-pyridine-2-carboxylic acid methylamide phenylsulfonate수율 69%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

The compound of example 1 as a free base (2.25 g) was suspended in ethanol (50 mL) and benzensulfonic acid (0.737 g) in ethanol (50 mL) was added. The mixture was heated with vigorous stirring. All solid material dissolved to give a reddish solution. The solution was allowed to cool to room temperature and the flask scratched. Crystal formation was difficult to achieve, some seeds were found, added to solution and placed in freezer overnight. Grayish-tan solids had formed in the flask; the material was broken up & collected by suction filtration. The solids were washed with ethanol, then hexane and air-dried. Weighed product: 2.05 g, 69% yield.

후처리

  1. temperatureThe mixture was heated with vigorous stirring
  2. dissolutionAll solid material dissolved
  3. customto give a reddish solution
  4. additionadded to solution
  5. customhad formed in the flask
  6. filtrationcollected by suction filtration
  7. washThe solids were washed with ethanol
  8. dry with materialhexane and air-dried

출처 및 근거

ORD 기록
ord-e81adf21d6f54daa937e6ac553879038
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637553B2

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