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Lithium Hydroxide → HCID 11189779, 화합물

HRID 1393111
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HRID 1393111 반응식
C[O:2][C:3](=[O:31])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([NH:12][CH2:13][C:14]2[S:18][C:17]([C:19]3[CH:24]=[CH:23][C:22]([C:25]([F:28])([F:27])[F:26])=[CH:21][CH:20]=3)=[N:16][C:15]=2[CH3:29])=[CH:8][C:7]=1[CH3:30].[Li+].[OH-]>C1COCC1.C(O)C>[CH3:30][C:7]1[CH:8]=[C:9]([NH:12][CH2:13][C:14]2[S:18][C:17]([C:19]3[CH:24]=[CH:23][C:22]([C:25]([F:27])([F:26])[F:28])=[CH:21][CH:20]=3)=[N:16][C:15]=2[CH3:29])[CH:10]=[CH:11][C:6]=1[O:5][CH2:4][C:3]([OH:31])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 69220462HCID 69220462, 화합물

생성물 1

HCID 11189779HCID 11189779, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of (2-methyl-4-{[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethyl]-amino}-phenoxy)-acetic acid methyl ester (330 mg, 0.73 mmol) in THF (2.2 ml) and ethanol (2.2 ml) was treated at 0° C. with 1N LiOH (2.2 ml) and stirred for 1.25 h at RT. The reaction was extracted with aqueous 10% KHSO4/Et2O (3×). The organic phase was washed with aqueous 10% NaCl, dried over Na2SO4 and evaporated. The product was crystallized from CH2Cl2/Et2O to give pure (2-methyl-4-{[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethyl]-amino}-phenoxy)-acetic acid, MS: 437.4 (MH)+, MP: 201-203° C., dec.

후처리

  1. extractionThe reaction was extracted with aqueous 10% KHSO4/Et2O (3×)
  2. washThe organic phase was washed with aqueous 10% NaCl
  3. dry with materialdried over Na2SO4
  4. customevaporated
  5. customThe product was crystallized from CH2Cl2/Et2O

출처 및 근거

ORD 기록
ord-9bf7488f23c94f0fa069d8fb2fbecfd8
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07345067B2

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