Sodium Carbonate → HCID 19004338, 화합물

HRID 2225811노트

반응식

HRID 2225811 반응식
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

참가 물질

5

반응물 2

HCID 10340Sodium CarbonateHCID 54295833HCID 54295833, 화합물

생성물 1

HCID 19004338HCID 19004338, 화합물수율 46.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-11e5920cba7d4f5ab6a68b7f11096c56
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344843

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