Sodium Hydroxide → 1-hydroxy-6-methoxy-1,3-diphenyl-1H-indene-2-carboxylic acid

HRID 19541

反応式

HRID 19541 の反応式
C([O:3][C:4]([C:6]1[C:7]([OH:29])([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:8]2[C:13]([C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[CH:12][CH:11]=[C:10]([O:21][CH3:22])[CH:9]=2)=[O:5])C.[OH-].[Na+]>C1COCC1.C(O)C>[OH:29][C:7]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:8]2[C:13](=[CH:12][CH:11]=[C:10]([O:21][CH3:22])[CH:9]=2)[C:14]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[C:6]1[C:4]([OH:5])=[O:3]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 115961681-hydroxy-6-methoxy-1,3-diphenyl-1H-indene-2-carboxylic acid ethyl ester

生成物 1

HCID 115305531-hydroxy-6-methoxy-1,3-diphenyl-1H-indene-2-carboxylic acid収率 97%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1-Hydroxy-6-methoxy-1,3-diphenyl-1H-indene-2-carboxylic acid ethyl ester (110 mg, 0.285 mmol) prepared in Example 1 was dissolved in THF, and an excess amount of sodium hydroxide dissolved in aqueous ethanol was added thereto in such a way not to cause layer separation. The mixture was stirred for 24 hrs at RT, and the pH was adjusted to 3˜4 using 2N hydrochloric acid. The resulting mixture was extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure, to obtain 99 mg of the titled compound (yield: 97%).

後処理

  1. additionwas added
  2. customlayer separation
  3. extractionThe resulting mixture was extracted with ethyl acetate
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous MgSO4
  6. concentrationconcentrated under a reduced pressure

出典と根拠

ORDレコード
ord-78fa1c3f82fa4aa1ad308a7ac05a1e66
出典データセット
uspto-grants-2010_06
特許番号
US07745439B2

関連ノート

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