Sodium Bicarbonate → HCID 85787172、化合物

HRID 644437ノート

反応式

HRID 644437 の反応式
Br[CH:2]([C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[C:3](=O)[C:4]([CH3:7])([CH3:6])[CH3:5].[NH2:15][C:16]([NH2:18])=[S:17].C(=O)([O-])O.[Na+]>C(O)C>[NH2:18][C:16]1[S:17][C:2]([C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[C:3]([C:4]([CH3:7])([CH3:6])[CH3:5])[N:15]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 546382Bromo-dipivaloylmethaneHCID 2723790Thiourea

生成物 1

HCID 85787172HCID 85787172、化合物収率 94.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-bromo-2,2,6,6-tetramethyl-3,5-heptanedione(α-bromo-dipivaloylmethane; 1.42 g, 5.40 mmol), thiourea (451.8 mg, 5.94 mmol) and ethanol (15 mL) was refluxed for 2 hours. After cooling, the reaction mixture was poured into saturated aqueous sodium hydrogen carbonate and extracted with ethyl acetate. After the organic layer was washed with water and brine, dried over anhydrous sodium sulfate, the residue obtained by evaporation under reduced pressure was crystallized (dichloromethane/hexane) to give the title compound (1.23 g, 94.5%) as a white crystal.

後処理

  1. temperaturewas refluxed for 2 hours
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washAfter the organic layer was washed with water and brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe residue obtained by evaporation under reduced pressure
  7. customwas crystallized (dichloromethane/hexane)

出典と根拠

ORDレコード
ord-10fbf1029112408bb89b4c1f251b2886
出典データセット
uspto-grants-2010_04
特許番号
US07700655B2

反応ノート

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