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Potassium Carbonate → HCID 23663550、化合物

HRID 1714427
ノート
印刷プレビュー

反応式

HRID 1714427 の反応式
[CH2:1]([O:5][CH2:6][C@@H:7]([NH:12][C:13]([C@H:15]1[O:17][C@@H:16]1[C:18]([OH:20])=[O:19])=[O:14])[CH2:8][CH:9]([CH3:11])[CH3:10])[CH:2]([CH3:4])[CH3:3].C(=O)([O-])[O-].[K+:25].[K+]>CC(C)=O.O>[CH2:1]([O:5][CH2:6][C@@H:7]([NH:12][C:13]([C@H:15]1[O:17][C@@H:16]1[C:18]([O-:20])=[O:19])=[O:14])[CH2:8][CH:9]([CH3:11])[CH3:10])[CH:2]([CH3:3])[CH3:4].[K+:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 9927318VEL-0230 free acid

生成物 1

HCID 23663550HCID 23663550、化合物収率 163.7%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒3 回HCID 962Water溶媒

実験手順

The (2S,3S)-3-[[(1S)-1-isobutoxymethyl-3-methylbutyl]carbamoyl]oxirane-2-carboxylic acid (4.83 g) prepared in Example 6 or 7 was dissolved in acetone (23 mL), and potassium carbonate (1.11 g) dissolved in water (4.5 mL) was slowly added. The solution was stirred at room temperature until the deposited inorganic salt was dissolved. While the solution was heated at 50° C. in a bath, acetone (100 mL) was dropped and a seed crystal was placed in the solution, and then the solution was stirred for 30 minutes. Acetone (94 mL) was again dropped, and the solution was stirred for 1 hour while the temperature was kept. While gradually cooled to room temperature, the solution was stirred overnight. The precipitated crystalline product was collected by filtration, washed with a mixture of 2% water-acetone (20 mL), dried in air to obtain white solid potassium (2S,3S)-3-[[(1S)-1-isobutoxymethyl-3-methylbutyl]carbamoyl]oxirane-2-carboxylate (4.28 g, 81.7%). The NMR data of the solid product were the same as those in Example 11.

後処理

  1. additionwas slowly added
  2. dissolutionwas dissolved
  3. temperatureWhile the solution was heated at 50° C. in a bath
  4. stirringthe solution was stirred for 30 minutes
  5. stirringthe solution was stirred for 1 hour while the temperature
  6. temperatureWhile gradually cooled to room temperature
  7. stirringthe solution was stirred overnight
  8. filtrationThe precipitated crystalline product was collected by filtration
  9. washwashed with a mixture of 2% water-acetone (20 mL)
  10. customdried in air

出典と根拠

ORDレコード
ord-bbd06477b73c456babab1e3c971f75a5
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795458B2

反応ノート

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