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

HRID 2094270노트

반응식

HRID 2094270 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-a88fc949b2284269a6e7470c66b343ed
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445525B2

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