Sodium Carbonate → VEL-0230

HRID 1714426ノート

反応式

HRID 1714426 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-].[Na+:25].[Na+]>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].[Na+:25]

参加物

5

反応物 2

HCID 10340Sodium CarbonateHCID 9927318VEL-0230 free acid

生成物 1

HCID 25102841VEL-0230収率 185.6%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒3 回HCID 962Water溶媒

実験手順

(2S,3S)-3-[[(1S)-1-isobutoxymethyl-3-methylbutyl]-carbamoyl]oxirane-2-carboxylic acid (48.59 g) was dissolved in acetone (245 mL), and sodium carbonate (8.51 g) dissolved in water (32.9 mL) was slowly added. The solution was stirred at room temperature to 50° C. for three hours until the deposited inorganic salt was dissolved. While the temperature was kept, acetone (200 mL) was dropped and a seed crystal was placed in the solution, and then the solution was stirred for 30 minutes. Acetone (510 mL) was again dropped, and the solution was stirred for 1 hour while the temperature was kept. While the solution was gradually cooled to room temperature, it was stirred overnight. The precipitated crystalline product was collected by filtration, washed with a mixture of 3% water-acetone (70 mL), dried in air to obtain white solid sodium (2S,3S)-3-[[(1S)-1-isobutoxymethyl-3-methylbutyl]carbamoyl]oxirane-2-carboxylate (46.1 g, 87.9%). The NMR data of the solid product were the same as those in Example 9.

後処理

  1. additionwas slowly added
  2. dissolutionwas dissolved
  3. stirringthe solution was stirred for 30 minutes
  4. stirringthe solution was stirred for 1 hour while the temperature
  5. stirringit was stirred overnight
  6. filtrationThe precipitated crystalline product was collected by filtration
  7. washwashed with a mixture of 3% water-acetone (70 mL)
  8. customdried in air

出典と根拠

ORDレコード
ord-fbe3664c4d394f88a44c459091080d6f
出典データセット
uspto-grants-2010_09
特許番号
US07795458B2

反応ノート

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