1,3-Dichloroacetone → HCID 57423799, 화합물

HRID 1869505노트

반응식

HRID 1869505 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:11][CH:10]([C:12](=[S:14])[NH2:13])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:15][CH2:16][C:17]([CH2:19]Cl)=O.[O-]S([O-])(=O)=O.[Mg+2]>CC(C)=O>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH:10]([C:12]2[S:14][CH:19]=[C:17]([CH2:16][Cl:15])[N:13]=2)[CH2:11]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 107931,3-DichloroacetoneHCID 24083Sulfuric acid magnesium salt (1:1)HCID 57473379Tert-butyl 3-carbamothioylazetidine-1-carboxylate

생성물 1

HCID 57423799HCID 57423799, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 3-Thiocarbamoyl-azetidine-1-carboxylic acid tert-butyl ester (0.800 g, 3.7 mmol) in acetone (15 mL) was added 1,3-dichloroacetone (0.611 g, 4.81 mmol), MgSO4 (0.67 g, 5.6 mmol) and MgCO3 (3.12 g, 3.7 mmol). The mixture was heated under reflux overnight, cooled and filtered through celite. The solvent was removed in vacuo and the residue was redissolved with EtOAc (20 mL). The resulting solution was washed successively with 5% NaHSO3, saturated NaHCO3, and brine. After drying (Na2SO4), the solvent was removed to afford the desired product which was used without further purification.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux overnight
  3. temperaturecooled
  4. filtrationfiltered through celite
  5. customThe solvent was removed in vacuo
  6. dissolutionthe residue was redissolved with EtOAc (20 mL)
  7. washThe resulting solution was washed successively with 5% NaHSO3, saturated NaHCO3, and brine
  8. dry with materialAfter drying (Na2SO4)
  9. customthe solvent was removed

출처 및 근거

ORD 기록
ord-b1b5964827154e46882889b7897379ce
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638541B2

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