Anisole → HCID 178481638, 화합물

HRID 1465980

반응식

HRID 1465980 반응식
[Al+3].[Cl-].[Cl-].[Cl-].COC1C=CC(C[N:12]2[C:17]3[NH:18][N:19]=[C:20]([NH:21][C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[C:16]=3[C:15](=[O:28])[N:14]([CH3:29])[C:13]2=[O:30])=CC=1.C1(OC)C=CC=CC=1>ClCCCl>[CH3:29][N:14]1[C:15](=[O:28])[C:16]2[C:20]([NH:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:19][NH:18][C:17]=2[NH:12][C:13]1=[O:30]

참가 물질

5

반응물 3

HCID 7519AnisoleHCID 6451240Aluminum(III) ChlorideHCID 178490875HCID 178490875, 화합물

생성물 1

HCID 178481638HCID 178481638, 화합물수율 99.8%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

AlCl3 (0.733 g, 5.50 mmol) is added to a solution of 7-(4-methoxybenzyl)-5-methyl-3-(phenylamino)-1H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (0.692 g, 1.83 mmol) and anisole (40 μL, 0.367 mmol) in 1,2-dichloroethane (10 mL) under argon. The reaction mixture is stirred at room temperature for 30 min, and then quenched with water with cooling. The resulting suspension is filtered through a layer of celite and the celite is washed with MeOH (20 mL). The product is eluted from the celite with a large amount of THF. The THF eluent is evaporated to afford 0.47 g of product (Yield: 99%). MS (FAB) m/z 258.2 [M+H]+.

후처리

  1. customquenched with water
  2. temperaturewith cooling
  3. filtrationThe resulting suspension is filtered through a layer of celite and the celite
  4. washis washed with MeOH (20 mL)
  5. washThe product is eluted from the celite with a large amount of THF
  6. customThe THF eluent is evaporated

출처 및 근거

ORD 기록
ord-8f477f58bfaa4198817a3a9be840ea8c
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09000001B2

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