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Methanol → 1-(4-Methyl-pyridin-3-yl)-3-thieno[3,2-c]pyridin-3-yl-imidazolidin-2-one

HRID 2383859
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HRID 2383859 반응식
Cl[C:2]1[C:7]2[C:8]([N:11]3[CH2:15][CH2:14][N:13]([C:16]4[CH:17]=[N:18][CH:19]=[CH:20][C:21]=4[CH3:22])[C:12]3=[O:23])=[CH:9][S:10][C:6]=2[CH:5]=[CH:4][N:3]=1.CO>C(O)(=O)C.C(Cl)Cl.[Zn]>[CH3:22][C:21]1[CH:20]=[CH:19][N:18]=[CH:17][C:16]=1[N:13]1[CH2:14][CH2:15][N:11]([C:8]2[C:7]3[CH:2]=[N:3][CH:4]=[CH:5][C:6]=3[S:10][CH:9]=2)[C:12]1=[O:23]
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참가 물질

6

반응물 2

HCID 887MethanolHCID 498722521-(4-Chloro-thieno[3,2-c]pyridin-3-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

생성물 1

HCID 596362761-(4-Methyl-pyridin-3-yl)-3-thieno[3,2-c]pyridin-3-yl-imidazolidin-2-one수율 40.6%

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 176Acetic Acid용매
HCID 6344
Dichloromethane
용매

실험 절차

Activated Zinc (417 mg, 6.380 mmol) was added to a stirred solution of 1-(4-chloro-thieno[3,2-c]pyridin-3-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (I-136a: 220 mg, 0.6380 mmol) in acetic acid (10 mL). The resulting mixture was stirred at room temperature for 2 days. The reaction was monitored by TLC (10% MeOH in DCM). The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. Aqueous NH3 solution was added to the concentrate and extracted with DCM. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford the crude product. Purification by column chromatography on silica gel (5% MeOH in DCM) afforded 80 mg of the product (40.6% yield).

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionAqueous NH3 solution was added to the
  4. concentrationconcentrate
  5. extractionextracted with DCM
  6. dry with materialThe organic layer was dried over Na2SO4
  7. concentrationconcentrated under reduced pressure
  8. customto afford the crude product
  9. customPurification by column chromatography on silica gel (5% MeOH in DCM)

출처 및 근거

ORD 기록
ord-bb2ba929d53b4fac8d2862145db13e09
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08263635B2

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