Aluminum(III) Chloride → HCID 25012028, 화합물

HRID 13051노트

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HRID 13051 반응식
[F:1][C:2]([F:35])([F:34])[C:3]([NH:5][C@@H:6]([CH3:33])[C@H:7]([O:16][C:17]1[CH:18]=[C:19]2[C:23](=[CH:24][CH:25]=1)[N:22]([C:26]1[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=1)[N:21]=[CH:20]2)[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14]C)[CH:9]=1)=[O:4].[Cl-].[Al+3].[Cl-].[Cl-]>CC1C=CC=CC=1>[F:34][C:2]([F:1])([F:35])[C:3]([NH:5][C@@H:6]([CH3:33])[C@H:7]([O:16][C:17]1[CH:18]=[C:19]2[C:23](=[CH:24][CH:25]=1)[N:22]([C:26]1[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=1)[N:21]=[CH:20]2)[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([OH:14])[CH:9]=1)=[O:4]

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 24825740AZD-5423

생성물 1

HCID 25012028HCID 25012028, 화합물수율 42.2%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
40 °C

실험 절차

To a stirred solution of 2,2,2-trifluoro-N-((1R,2S)-1-(1-(4-fluorophenyl)-1H-indazol-5-yloxy)-1-(3-methoxyphenyl)propan-2-yl)acetamide (Example 6, 10 mg, 20 μmol) in methylbenzene (1 ml) was added dodecanethiole (1 ml), followed with anhydrous aluminium chloride (5.3 mg, 40 μmol). The mixture was stirred at 40° C. for 1 h. Methylbenzene was removed in vacuo, the solution in dodecanethiole was diluted with n-heptane (10 ml). Oily precipitate has formed, which was washed with heptane, dried in vacuo, and dissolved in acetonitrile/water mixture. The crude product was purified by preparative HPLC afforded 4 mg of product as a white solid (42%).

후처리

  1. customMethylbenzene was removed in vacuo
  2. additionthe solution in dodecanethiole was diluted with n-heptane (10 ml)
  3. customOily precipitate has formed
  4. washwhich was washed with heptane
  5. customdried in vacuo
  6. dissolutiondissolved in acetonitrile/water mixture
  7. customThe crude product was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-0099cb2593d64fb4bcefdf71a5a06ba3
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728030B2

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