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

HRID 2383859
ノート
印刷プレビュー

反応式

HRID 2383859 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-bb2ba929d53b4fac8d2862145db13e09
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263635B2

反応ノート

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