1,3-Dichloroacetone → HCID 57423801、化合物

HRID 2063436ノート

反応式

HRID 2063436 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([C:14](=[S:16])[NH2:15])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:17][CH2:18][C:19]([CH2:21]Cl)=O.[O-]S([O-])(=O)=O.[Mg+2]>CC(C)=O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([C:14]2[S:16][CH:21]=[C:19]([CH2:18][Cl:17])[N:15]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 107931,3-DichloroacetoneHCID 24083Sulfuric acid magnesium salt (1:1)HCID 23546083tert-Butyl 3-carbamothioylpiperidine-1-carboxylate

生成物 1

HCID 57423801HCID 57423801、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 3-Thiocarbamoyl-piperidine-1-carboxylic acid tert-butyl ester (2.2 g, 9.02 mmol) in acetone (45 mL) was added 1,3-dichloroacetone (1.49 g, 11 7 mmol), MgSO4 (1.63 g, 13.5 mmol) and MgCO3 (0.76 g, 9.02 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.

後処理

  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

出典と根拠

ORDレコード
ord-5c0164f2310c4b799a7663c24754e68a
出典データセット
uspto-grants-2012_10
特許番号
US08288384B2

反応ノート

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