Hydrochloric Acid → HCID 57559703, 화합물

HRID 1723956노트

반응식

HRID 1723956 반응식
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([C:11]2[CH:16]=[C:15]([C:17](=[O:36])[NH:18][C:19]3[CH:24]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:22]=[C:21]([NH:29][S:30]([CH3:33])(=[O:32])=[O:31])[C:20]=3[O:34][CH3:35])[CH:14]=[CH:13][C:12]=2[CH3:37])[CH:10]=1)=[O:5])C.[OH-].[Na+].Cl>CO>[C:25]([C:23]1[CH:22]=[C:21]([NH:29][S:30]([CH3:33])(=[O:31])=[O:32])[C:20]([O:34][CH3:35])=[C:19]([NH:18][C:17]([C:15]2[CH:14]=[CH:13][C:12]([CH3:37])=[C:11]([N:9]3[CH:10]=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]3)[CH:16]=2)=[O:36])[CH:24]=1)([CH3:28])([CH3:26])[CH3:27]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 11685140HCID 11685140, 화합물

생성물 1

HCID 57559703HCID 57559703, 화합물수율 91.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1-[5-(5-tert-butyl-3-methanesulfonylamino-2-methoxy-phenylcarbamoyl)-2-methyl-phenyl]-1H-pyrazole-4-carboxylic acid ethyl ester (Example 2) (900 mg) was suspended in MeOH (7 mL). A solution of 10% sodium hydroxide (33 mL) was added and the reaction stirred 2 h. The solution was acidified with concentrated HCl to a pH of 4 resulting in a suspension. The suspension was cooled in an ice bath and the solids collected by vacuum filtration. The solids were washed with water, dried under vacuum over P2O5 at 50° C. to provide 1-[5-(5-tert-butyl-3-methanesulfonylamino-2-methoxy-phenylcarbamoyl)-2-methyl-phenyl]-1H-pyrazole-4-carboxylic acid (782 mg, 91%) as a white solid.

후처리

  1. customresulting in a suspension
  2. temperatureThe suspension was cooled in an ice bath
  3. filtrationthe solids collected by vacuum filtration
  4. washThe solids were washed with water
  5. dry with materialdried under vacuum over P2O5 at 50° C.

출처 및 근거

ORD 기록
ord-8064ad693dd0445aa43d35a5a3d0a21f
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07485657B2

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