Hydrochloric Acid → HCID 68996058, 화합물

HRID 578815노트

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HRID 578815 반응식
C[O:2][C:3]([C:5]1[S:6][CH:7]=[C:8]2[C:13]=1[C:12](=[O:14])[N:11]([C:15]1[CH:20]=[C:19]([C:21](=[O:30])[N:22]([CH3:29])[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:18]=[CH:17][C:16]=1[F:31])[C:10](=[O:32])[NH:9]2)=[O:4].O.[OH-].[Li+].CO.Cl>O1CCCC1.O>[C:3]([C:5]1[S:6][CH:7]=[C:8]2[C:13]=1[C:12](=[O:14])[N:11]([C:15]1[CH:20]=[C:19]([C:21](=[O:30])[N:22]([CH3:29])[C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:18]=[CH:17][C:16]=1[F:31])[C:10](=[O:32])[NH:9]2)([OH:4])=[O:2]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 58022073HCID 58022073, 화합물

생성물 1

HCID 68996058HCID 68996058, 화합물수율 68.8%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 5-methoxycarbonyl-3-[2-fluoro-5-(N -methyl-N-phenylcarbamoyl) phenyl]thieno[3,4-d]pyrimidine -2,4(1H,3H)-dione (0.18 g) and lithium hydroxide-monohydrate (0.17 g) in tetrahydrofuran (6 mL)-methanol (3 mL)-water (3 mL) was stirred at room temperature for 2 hours. The reaction mixture was poured into 1 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with brine and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: methylene chloride/methanol=8/1) to give the title compound (0.12 g).

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: methylene chloride/methanol=8/1)

출처 및 근거

ORD 기록
ord-ed1f5095802148bdb267ee4cc23b0957
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040693B2

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