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Sodium Hydroxide → HCID 60053887, 화합물

HRID 34136
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HRID 34136 반응식
C[O:2][C:3]([C:5]1([NH:8][C:9]([C:11]2[C:12]([O:29][CH3:30])=[C:13]3[C:17](=[CH:18][CH:19]=2)[NH:16][N:15]=[C:14]3/[CH:20]=[CH:21]/[C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)=[O:10])[CH2:7][CH2:6]1)=[O:4].[OH-].[Na+]>O1CCCC1.CO.O>[F:28][C:25]1[CH:24]=[CH:23][C:22](/[CH:21]=[CH:20]/[C:14]2[C:13]3[C:17](=[CH:18][CH:19]=[C:11]([C:9]([NH:8][C:5]4([C:3]([OH:4])=[O:2])[CH2:7][CH2:6]4)=[O:10])[C:12]=3[O:29][CH3:30])[NH:16][N:15]=2)=[CH:27][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 14798Sodium HydroxideHCID 60053859methyl 1-[[3-[(E)-2-(4-fluorophenyl)ethenyl]-4-methoxy-1H-indazole-5-carbonyl]amino]cyclopropane-1-carboxylate

생성물 1

HCID 60053887HCID 60053887, 화합물수율 78.2%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

To a mixed solution of 200 mg of 1-({3-[(E)-2-(4-fluorophenyl)-vinyl]-4-methoxy-1H-indazol-5-carbonyl}-amino)-cyclopropane carboxylic acid methyl ester obtained in Example 1317 in 5 ml of tetrahydrofuran and 2 ml of methanol was added 2 ml of a 1N sodium hydroxide aqueous solution, followed by stirring at room temperature overnight. The reaction mixture was diluted with water and the aqueous layer was washed with diethyl ether. The aqueous layer was adjusted to pH 2 by adding 1N hydrochloric acid, and the precipitated solid was collected by filtration with glass filter. The solid was washed with water and was dried under reduced pressure, to give 151 mg of the title compound as a brown solid.

후처리

  1. washthe aqueous layer was washed with diethyl ether
  2. additionby adding 1N hydrochloric acid
  3. filtrationthe precipitated solid was collected by filtration with glass
  4. filtrationfilter
  5. washThe solid was washed with water
  6. customwas dried under reduced pressure

출처 및 근거

ORD 기록
ord-bf3fc7c1c15c4d7580136665173122ab
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07429609B2

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