Hydrochloric Acid → HCID 22251491、化合物

HRID 1264354ノート

反応式

HRID 1264354 の反応式
C[O:2][C:3](=[O:20])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12](=[O:19])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:6][CH:5]=1.[Li+].[OH-].Cl>O.C1COCC1>[O:19]=[C:12]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:11][CH2:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([OH:20])=[O:2])=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 18618679HCID 18618679、化合物

生成物 1

HCID 22251491HCID 22251491、化合物

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

To a solution of methyl ester 47 (195 mg, 0.73 mmol) in water/THF (1:1, 0.07M) was added LiOH (46 mg, 1.1 mmol). The resulting solution was stirred overnight at room temperature or until no starting material was detected by TLC. HCl 1N was added and the solution was extracted with EtOAc and the organic layer was dried over anhydrous MgSO4. Filtration and evaporation of the solvent under vacuum followed by purification by column chromatography using 10% MeOH/CH2Cl2, gave the title compound.

後処理

  1. extractionthe solution was extracted with EtOAc
  2. dry with materialthe organic layer was dried over anhydrous MgSO4
  3. filtrationFiltration and evaporation of the solvent under vacuum
  4. customfollowed by purification by column chromatography

出典と根拠

ORDレコード
ord-3f394f95063044c79989c7f2239ecea6
出典データセット
uspto-grants-2003_04
特許番号
US06541661B1

反応ノート

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