HCID 11173633, 화합물 → HCID 9958096, 화합물

HRID 2214758

반응식

HRID 2214758 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 9958096HCID 9958096, 화합물수율 82%

시약·촉매·용매 1

HCID 1140Toluene용매3회

반응 조건

온도
90 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-070a8aed011e44258801dc36598743b2
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07109201B2

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