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Water → 4-Chloro-5-methoxy-7-iodoisoindolinone

HRID 21246
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인쇄 미리보기

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HRID 21246 반응식
[Cl:1][C:2]1[C:10]([O:11][CH3:12])=[CH:9][C:8]([I:13])=[C:7]2[C:3]=1[CH:4](O)[N:5](C(C)(C1C=CC=CC=1)C)[C:6]2=[O:14].FC(F)(F)C(O)=O.C([SiH](CC)CC)C.O>[N+](C)([O-])=O.CCCCCC.C(OCC)(=O)C>[Cl:1][C:2]1[C:10]([O:11][CH3:12])=[CH:9][C:8]([I:13])=[C:7]2[C:3]=1[CH2:4][NH:5][C:6]2=[O:14]
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참가 물질

8

반응물 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 684892124-Chloro-5-methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone

생성물 1

HCID 684924484-Chloro-5-methoxy-7-iodoisoindolinone수율 64.2%

시약·촉매·용매 3

HCID 6375
Nitromethane
용매
HCID 8058Hexane용매
HCID 8857Ethyl Acetate용매

실험 절차

In a similar manner to Step 4 of Example 16, 4-chloro-5-methoxy-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (300 mg, 0.655 mmol) was dissolved in nitromethane (5 mL), and the solution was treated with trifluoroacetic acid (0.505 mL, 6.55 mmol) and triethylsilane (0.212 mL, 1.31 mmol), followed by stirring at room temperature for 24 hours. The reaction mixture was added with water, ethyl acetate and hexane. The precipitated solid was collected by filtration and washed with hexane and water, followed by drying under reduced pressure to obtain 4-chloro-5-methoxy-7-iodoisoindolinone (136 mg, yield 64%).

후처리

  1. filtrationThe precipitated solid was collected by filtration
  2. washwashed with hexane and water
  3. customby drying under reduced pressure

출처 및 근거

ORD 기록
ord-dd693a902a3342af89c07ffd9aa57680
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745641B2

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