Hydrochloric Acid → HCID 68996058、化合物

HRID 578815ノート

反応式

HRID 578815 の反応式
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]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 58022073HCID 58022073、化合物

生成物 1

HCID 68996058HCID 68996058、化合物収率 68.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-ed1f5095802148bdb267ee4cc23b0957
出典データセット
uspto-grants-2015_05
特許番号
US09040693B2

反応ノート

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