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

HRID 19541

반응식

HRID 19541 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-78fa1c3f82fa4aa1ad308a7ac05a1e66
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745439B2

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