Water → Methyl 4-(1,1-dioxo-isothiazolidin-2-yl)-3-methyl-benzoate

HRID 1629840ノート

反応式

HRID 1629840 の反応式
Cl[CH2:2][CH2:3][CH2:4][S:5]([NH:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][C:10]=1[CH3:19])(=[O:7])=[O:6].[K].CC(C)([O-])C.O>CN(C=O)C>[O:6]=[S:5]1(=[O:7])[CH2:4][CH2:3][CH2:2][N:8]1[C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][C:10]=1[CH3:19]

参加物

5

反応物 3

HCID 962WaterHCID 43654282Methyl 4-(3-chloro-propyl-sulphonyl-amino)-3-methyl-benzoateHCID 50987170Potassium tertbutoxide

生成物 1

HCID 67048536Methyl 4-(1,1-dioxo-isothiazolidin-2-yl)-3-methyl-benzoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

370 mg (0.85 mmol) 70% methyl 4-(3-chloropropane-sulphonylamino)-3-methyl-benzoate dissolved in 26 ml DMF are combined with 275 mg (2.45 mmol) potassium-tert.-butoxide and stirred for 16 hours at ambient temperature. The reaction mixture is combined with water and extracted with ethyl acetate. The combined organic phases are dried over sodium sulphate, evaporated down i. vac. and the residue is purified by chromatography on silica gel (eluant: dichloromethane/isopropanol 98:2).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic phases are dried over sodium sulphate
  3. customevaporated down i
  4. customand the residue is purified by chromatography on silica gel (eluant: dichloromethane/isopropanol 98:2)

出典と根拠

ORDレコード
ord-2c953683536645e6b58e8d95019abddc
出典データセット
uspto-grants-2014_07
特許番号
US08791103B2

反応ノート

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