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Water → HCID 178437880, 화합물

HRID 1600795
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HRID 1600795 반응식
[Na].[CH:2]1([N:7]2[C:11]([NH2:12])=[C:10]([C:13]([NH2:15])=[O:14])[C:9]([CH2:16][CH3:17])=[N:8]2)[CH2:6][CH2:5][CH2:4][CH2:3]1.[N:18]1([CH2:24][CH2:25][O:26][C:27]2[CH:32]=[CH:31][C:30]([CH2:33][C:34](OC)=O)=[CH:29][CH:28]=2)[CH2:23][CH2:22][O:21][CH2:20][CH2:19]1.O>C(O)C.CCOCC.C(O)(=O)C>[CH:2]1([N:7]2[C:11]3=[N:12][C:34]([CH2:33][C:30]4[CH:31]=[CH:32][C:27]([O:26][CH2:25][CH2:24][N:18]5[CH2:23][CH2:22][O:21][CH2:20][CH2:19]5)=[CH:28][CH:29]=4)=[N:15][C:13](=[O:14])[C:10]3=[C:9]([CH2:16][CH3:17])[NH:8]2)[CH2:3][CH2:4][CH2:5][CH2:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 5360545SodiumHCID 21830903Methyl 4-[2-(4-morpholinyl)ethoxy]phenylacetateHCID 224493525-amino-1-cyclopentyl-3-ethyl-1H-pyrazole-4-carboxamide

생성물 1

HCID 178437880HCID 178437880, 화합물수율 41.1%

시약·촉매·용매 3

HCID 176
Acetic Acid
용매
HCID 702Ethanol용매
HCID 3283Diethyl Ether용매

실험 절차

Sodium (414 mg) was dissolved in ethanol (30 ml) and 1-cyclopentyl-3-ethyl-5-amino-1H-pyrazole-4-carboxamide (2.0 g) and methyl 4-[2-(4-morpholinyl)ethoxy]phenylacetate (5.03 g, 18 mmol) were added. The reaction mixture was refluxed overnight, the solvent was stripped, water was added to the residue, followed by sufficient acetic acid to adjust the pH to 8-9. An oil separated which was collected by decantation and treated with water and saturated NaHCO3. The mixture was extracted with ethyl acetate and washed with water and then saturated NaHCO3 (2×). The aqueous layer was extracted with additional ethyl acetate and the combined organic layers were washed with 2N NaOH and brine. The organic layer was dried over MgSO4, filtered and stripped to afford crude product which was digested with ether and collected by filtration. The crude product was purified by several acid/base work-ups, followed by recrystallization from ether to afford 1.67 g of 1-cyclopentyl-3-ethyl-6-[4-[2-(4-morpholinyl)ethoxy]phenylmethyl]pyrazolo[3,4-d]pyrimidin-4-one, m.p. 136-137° C.

후처리

  1. temperatureThe reaction mixture was refluxed overnight
  2. customAn oil separated which
  3. customwas collected by decantation
  4. additiontreated with water and saturated NaHCO3
  5. extractionThe mixture was extracted with ethyl acetate
  6. washwashed with water
  7. extractionThe aqueous layer was extracted with additional ethyl acetate
  8. washthe combined organic layers were washed with 2N NaOH and brine
  9. dry with materialThe organic layer was dried over MgSO4
  10. filtrationfiltered
  11. customto afford crude product which
  12. filtrationcollected by filtration
  13. customThe crude product was purified by several acid/base work-ups
  14. customfollowed by recrystallization from ether

출처 및 근거

ORD 기록
ord-3d49753fd5744dc98b82fe5877d3cf97
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05977118

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