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Acetic Acid → Acetic acid 8-cyclopentyl-2-methylsulfanyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-6-ylmethyl ester

HRID 272437
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HRID 272437 반응식
Br[CH2:2][C:3]1[C:14](=[O:15])[N:13]([CH:16]2[CH2:20][CH2:19][CH2:18][CH2:17]2)[C:6]2[N:7]=[C:8]([S:11][CH3:12])[N:9]=[CH:10][C:5]=2[CH:4]=1.[C:21]([OH:24])(=[O:23])[CH3:22]>C([O-])(=O)C.[Ag+]>[CH:16]1([N:13]2[C:6]3[N:7]=[C:8]([S:11][CH3:12])[N:9]=[CH:10][C:5]=3[CH:4]=[C:3]([CH2:2][O:24][C:21](=[O:23])[CH3:22])[C:14]2=[O:15])[CH2:20][CH2:19][CH2:18][CH2:17]1
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참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 111873396-bromomethyl-8-cyclopentyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 11348177Acetic acid 8-cyclopentyl-2-methylsulfanyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-6-ylmethyl ester수율 71%

시약·촉매·용매 1

HCID 11246Silver acetate촉매

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온도
110 °C

실험 절차

6-Bromomethyl-8-cyclopentyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one (1.33 g, 3.75 mmol), prepared as in Example 25, and silver acetate (1.03 g, 6.2 mmol) were added to glacial acetic acid (10 ml) and heated to 110° C. for 5 hours. The solvents then were evaporated at reduced pressure and the resulting residue was suspended in ethyl acetate and filtered. The solid obtained was recrystallized from ethyl acetate to provide acetic acid 8-cyclopentyl-2-methylsulfanyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-6-ylmethyl ester as a solid (0.89 g, 71%). MS (APCI) M++1; Calc'd 334.11. Found 334.2.

후처리

  1. customThe solvents then were evaporated at reduced pressure
  2. filtrationfiltered
  3. customThe solid obtained
  4. customwas recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-95e308c0e3f84c5cb627cbb6bcef294d
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07456168B2

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