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Lithium hydroxide, monohydrate → 4-[4-(4-Fluoro-2-methyl-1H-indol-5-yloxy)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid lithium salt

HRID 133055
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HRID 133055 반응식
C([O:3][C:4](=[O:32])[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[NH:31][C:14]3[N:15]=[CH:16][N:17]=[C:18]([O:19][C:20]4[C:21]([F:30])=[C:22]5[C:26](=[CH:27][CH:28]=4)[NH:25][C:24]([CH3:29])=[CH:23]5)[C:13]=3[CH:12]=2)=[CH:7][CH:6]=1)C.O[Li:34].O>O1CCOCC1.O>[Li+:34].[F:30][C:21]1[C:20]([O:19][C:18]2[C:13]3[CH:12]=[C:11]([C:8]4[CH:7]=[CH:6][C:5]([C:4]([O-:32])=[O:3])=[CH:10][CH:9]=4)[NH:31][C:14]=3[N:15]=[CH:16][N:17]=2)=[CH:28][CH:27]=[C:26]2[C:22]=1[CH:23]=[C:24]([CH3:29])[NH:25]2
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HCID 168937Lithium hydroxide, monohydrateHCID 691794854-[4-(4-Fluoro-2-methyl-1H-indol-5-yloxy)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid ethyl ester

생성물 1

HCID 691806194-[4-(4-Fluoro-2-methyl-1H-indol-5-yloxy)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid lithium salt

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane
용매

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온도
120 °C

실험 절차

A suspension of 2.87 g (6.7 mMol) of 4-[4-(4-fluoro-2-methyl-1H-indol-5-yloxy)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid ethyl ester and 520 mg (12 mMol) LiOH.H2O in 240 ml of dioxane and 5 ml of water is stirred for 24 h at 120° C. The solid is dissolved first, then a new precipitate is formed. Filtration at RT and washing with dioxane and diethylether gives the title compound; HPLC (conditions see Examples 67-78) tR=13.5 min; MS-ES+: (M+H)+=403.

후처리

  1. dissolutionThe solid is dissolved first
  2. customa new precipitate is formed
  3. filtrationFiltration at RT
  4. washwashing with dioxane and diethylether

출처 및 근거

ORD 기록
ord-6ae2146f34bc4989bba4594d2187ebab
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07390805B2

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