Triethylamine → Methanesulfonamide,n-[3-[(4-chloro-2,3-dihydro-7-iodo-1-oxo-1h-isoindol-5-yl)oxy]propyl]-

HRID 21315ノート

反応式

HRID 21315 の反応式
Cl.[Cl:2][C:3]1[C:11]([O:12][CH2:13][CH2:14][CH2:15][NH2:16])=[CH:10][C:9]([I:17])=[C:8]2[C:4]=1[CH2:5][NH:6][C:7]2=[O:18].C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>ClCCl>[Cl:2][C:3]1[C:11]([O:12][CH2:13][CH2:14][CH2:15][NH:16][S:27]([CH3:26])(=[O:29])=[O:28])=[CH:10][C:9]([I:17])=[C:8]2[C:4]=1[CH2:5][NH:6][C:7]2=[O:18]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 684884094-Chloro-5-(3-aminopropoxy)-7-iodoisoindolinone hydrochloride

生成物 1

HCID 68492844Methanesulfonamide,n-[3-[(4-chloro-2,3-dihydro-7-iodo-1-oxo-1h-isoindol-5-yl)oxy]propyl]-収率 47%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-Chloro-5-(3-aminopropoxy)-7-iodoisoindolinone hydrochloride (100 mg, 0.248 mmol) was suspended in dichloromethane (3.0 mL), and the suspension was added with triethylamine (0.104 mL, 0.744 mmol) and methanesulfonyl chloride (0.029 mL, 0.372 mmol), followed by stirring at room temperature for 13 hours. The solvent was evaporated under reduced pressure, and the residue was purified by slurry using water and acetonitrile to obtain 4-chloro-5-[3-(methanesulfonylamino)propoxy]-7-iodoisoindolinone (51.8 mg, yield 47%).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by slurry

出典と根拠

ORDレコード
ord-38d0b3e4e8f44f649fd85c9b6ec23f7d
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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