Sodium Carbonate → HCID 19004338、化合物

HRID 2225811ノート

反応式

HRID 2225811 の反応式
C([O:3][C:4](=[O:29])[C:5](=[O:28])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][C:14](=[O:27])[N:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:17][CH2:16]2)=[CH:8][CH:7]=1)C.C(=O)([O-])[O-].[Na+].[Na+]>CO.O>[O:27]=[C:14]([N:15]1[CH2:20][CH2:19][N:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:17][CH2:16]1)[CH2:13][O:12][C:9]1[CH:10]=[CH:11][C:6]([C:5](=[O:28])[C:4]([OH:29])=[O:3])=[CH:7][CH:8]=1

参加物

5

反応物 2

HCID 10340Sodium CarbonateHCID 54295833HCID 54295833、化合物

生成物 1

HCID 19004338HCID 19004338、化合物収率 46.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

4-[2-Oxo-2-(4-phenyl-1-piperazinyl)ethoxy]-alpha-oxobenzeneacetic acid ethyl ester (0.7 g) in methanol (40 mL) was treated with sodium carbonate (0.24 g) in water (6 mL), and the mixture was stirred at room temperature for 1.25 hours. After the methanol was evaporated under reduced pressure, water was added and the solution was acidified with 3N hydrochloric acid, then the aqueous layer was extracted with a dichloromethane-tetrahydrofuran mixture (1:1). The organic layer was dried (MgSO4), evaporated, and the residue was crystallized from acetone to furnish 0.3 g of 4-[2-oxo-2-(4-phenyl-1-piperazinyl)ethoxy]-alpha-oxobenzeneacetic acid, mp 188°-192 ° C.

後処理

  1. customAfter the methanol was evaporated under reduced pressure, water
  2. additionwas added
  3. extractionthe aqueous layer was extracted with a dichloromethane-tetrahydrofuran mixture (1:1)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. customevaporated
  6. customthe residue was crystallized from acetone

出典と根拠

ORDレコード
ord-11e5920cba7d4f5ab6a68b7f11096c56
出典データセット
uspto-grants-1994_09
特許番号
US05344843

反応ノート

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