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

HRID 21246
ノート
印刷プレビュー

反応式

HRID 21246 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

HCID 684924484-Chloro-5-methoxy-7-iodoisoindolinone収率 64.2%

試薬・触媒・溶媒 3

HCID 6375
Nitromethane
溶媒
HCID 8058Hexane溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-dd693a902a3342af89c07ffd9aa57680
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745641B2

反応ノート

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