Aluminum(III) Chloride → HCID 25012028、化合物

HRID 13051ノート

反応式

HRID 13051 の反応式
[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]

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 24825740AZD-5423

生成物 1

HCID 25012028HCID 25012028、化合物収率 42.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
40 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-0099cb2593d64fb4bcefdf71a5a06ba3
出典データセット
uspto-grants-2010_06
特許番号
US07728030B2

反応ノート

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