Water → HCID 86628297、化合物

HRID 21265ノート

反応式

HRID 21265 の反応式
[CH3:1][S:2]([O:5][C:6]1[C:14]([CH:15](OC)[O:16][CH3:17])=[CH:13][C:12]([I:20])=[C:11]2[C:7]=1[CH:8](OC)[N:9](C(C)(C1C=CC=CC=1)C)[C:10]2=[O:21])(=[O:4])=[O:3].FC(F)(F)C(O)=O.C([SiH](CC)CC)C.O>[N+](C)([O-])=O.CCCCCC.C(OCC)(=O)C>[CH3:1][S:2]([O:5][C:6]1[C:14]([CH2:15][O:16][CH3:17])=[CH:13][C:12]([I:20])=[C:11]2[C:7]=1[CH2:8][NH:9][C:10]2=[O:21])(=[O:3])=[O:4]

参加物

8

反応物 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 866282964-Methanesulfonyloxy-5-dimethoxymethyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone

生成物 1

HCID 86628297HCID 86628297、化合物収率 72.4%

試薬・触媒・溶媒 3

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

反応条件

温度
50 °C

実験手順

In a similar manner to Step 4 of Example 16, 4-methanesulfonyloxy-5-dimethoxymethyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (226 mg, 0.393 mmol) was dissolved in nitromethane (5 mL), and the solution was added with trifluoroacetic acid (0.775 mL, 10.1 mmol) and triethylsilane (0.406 mL, 2.51 mmol), followed by stirring at 50° C. for 1 hour. The reaction mixture was added with water, ethyl acetate and hexane. The precipitated solid was collected by filtration and washed with water, followed by drying under reduced pressure to obtain 4-methanesulfonyloxy-5-methoxymethyl-7-iodoisoindolinone (113 mg, yield 72%).

後処理

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

出典と根拠

ORDレコード
ord-576ef63e032743879434c13e7bc63fbb
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

反応ノート

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