HCID 11173633、化合物 → HCID 9958096、化合物

HRID 2214758ノート

反応式

HRID 2214758 の反応式
[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:17]=[C:16]3[C:12]([CH2:13][CH2:14][NH:15]3)=[CH:11][C:10]=2[O:18][CH3:19])[CH2:3]1.C[Al](C)C.[C:24]([NH:27][C:28]1[N:33]=[C:32]([CH3:34])[C:31]([C:35]2[CH:44]=[CH:43][C:38]([C:39](OC)=[O:40])=[CH:37][CH:36]=2)=[CH:30][CH:29]=1)(=[O:26])[CH3:25]>C1(C)C=CC=CC=1>[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:17]=[C:16]3[C:12]([CH2:13][CH2:14][N:15]3[C:39]([C:38]3[CH:37]=[CH:36][C:35]([C:31]4[CH:30]=[CH:29][C:28]([NH:27][C:24](=[O:26])[CH3:25])=[N:33][C:32]=4[CH3:34])=[CH:44][CH:43]=3)=[O:40])=[CH:11][C:10]=2[O:18][CH3:19])[CH2:3]1

参加物

5

反応物 3

HCID 11173633HCID 11173633、化合物HCID 11265480cis-6-(3,5-Dimethylpiperazin-1-yl)-5-methoxyindolineHCID 16682925Trimethylaluminum

生成物 1

HCID 9958096HCID 9958096、化合物収率 82%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

反応条件

温度
90 °C

実験手順

A stirred solution of D3 (40 mg, 150 umole) in toluene (2 ml) at room temperature under argon was treated with 2M trimethylaluminium in toluene (0.15 ml, 300 umole) and maintained for 15 min, then a solution of D7 (57 mg, 200 umole) in toluene (3 ml) was added and the mixture heated at 90° C. for 1 h. The solution was allowed to cool, then added directly to a silica gel column (5 g) and eluted initially with 2% MeOH/DCM to remove high Rf impurities, then with 10% MeOH/DCM to afford the product. This was triturated with Et2O/DCM to afford the title compound as a beige solid (35 mg, 82%).

後処理

  1. temperaturemaintained for 15 min
  2. temperatureto cool
  3. additionadded directly to a silica gel column (5 g)
  4. washeluted initially with 2% MeOH/DCM
  5. customto remove high Rf impurities
  6. customwith 10% MeOH/DCM to afford the product
  7. customThis was triturated with Et2O/DCM

出典と根拠

ORDレコード
ord-070a8aed011e44258801dc36598743b2
出典データセット
uspto-grants-2006_09
特許番号
US07109201B2

反応ノート

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