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Trifluoroacetic acid → 4-Hydroxy-5-methyl-7-iodoisoindolinone

HRID 21277
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반응식

HRID 21277 반응식
COC[O:4][C:5]1[C:13]([CH3:14])=[CH:12][C:11]([I:15])=[C:10]2[C:6]=1[CH:7](O)[N:8](C(C)(C1C=CC=CC=1)C)[C:9]2=[O:16].FC(F)(F)C(O)=O.C([SiH](CC)CC)C.C(=O)([O-])O.[Na+]>[N+](C)([O-])=O.C(OCC)(=O)C>[OH:4][C:5]1[C:13]([CH3:14])=[CH:12][C:11]([I:15])=[C:10]2[C:6]=1[CH2:7][NH:8][C:9]2=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 516892Sodium BicarbonateHCID 68490123HCID 68490123, 화합물

생성물 1

HCID 684874154-Hydroxy-5-methyl-7-iodoisoindolinone수율 52.1%

시약·촉매·용매 2

HCID 6375Nitromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

In a similar manner to Step. 4 of Example 16, 4-methoxymethoxy-5-methyl-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (500 mg, 1.07 mmol) was dissolved in nitromethane (20 mL), and the solution was treated with trifluoroacetic acid (0.742 mL, 9.63 mmol) and triethylsilane (1.54 mL, 9.64 mmol). The reaction mixture was added with saturated aqueous sodium hydrogencarbonate solution and ethyl acetate. The precipitated solid was collected by filtration and washed with water, followed by drying under reduced pressure to obtain 4-hydroxy-5-methyl-7-iodoisoindolinone (161 mg, yield 52%).

후처리

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

출처 및 근거

ORD 기록
ord-1e82547495c24af0a018eb52b19dc314
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745641B2

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