Triethylamine → HCID 89922461、化合物

HRID 921917ノート

反応式

HRID 921917 の反応式
[Cl:1][C:2]1[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH:10]([CH2:14][NH:15]CC3C=CC(OC)=CC=3)[CH2:9]2)=[CH:6][C:5]([C:25]#[N:26])=[CH:4][C:3]=1[NH:27][C:28]1[N:33]=[C:32]([N:34]([CH:44]2[CH2:46][CH2:45]2)CC2C=CC(OC)=CC=2)[C:31]2=[N:47][CH:48]=[C:49]([C:50]#[N:51])[N:30]2[N:29]=1.C(N(CC)CC)C.[CH3:59][S:60](Cl)(=[O:62])=[O:61].C(=O)(O)[O-].[Na+]>O1CCCC1.C(OCC)(=O)C>[Cl:1][C:2]1[C:3]([NH:27][C:28]2[N:33]=[C:32]([NH:34][CH:44]3[CH2:46][CH2:45]3)[C:31]3=[N:47][CH:48]=[C:49]([C:50]#[N:51])[N:30]3[N:29]=2)=[CH:4][C:5]([C:25]#[N:26])=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][NH:15][S:60]([CH3:59])(=[O:62])=[O:61])[CH2:9]1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 89923206(+/-)-2-((2-Chloro-5-cyano-3-(2-(((4-methoxybenzyl)amino)methyl)morpholino)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile

生成物 1

HCID 89922461HCID 89922461、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a round bottom flask charged with (+/−)-2-((2-chloro-5-cyano-3-(2-(((4-methoxybenzyl)amino)methyl)morpholino)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (38.9 mg, 0.055 mmol) in tetrahydrofuran (276 μl) was added triethylamine (13.84 μl, 0.099 mmol) and methanesulfonyl chloride (5.59 μl, 0.072 mmol). The reaction mixture was stirred at room temperature ON. The reaction mixture was diluted with ethyl acetate and transferred to a separatory funnel containing saturated aqueous sodium bicarbonate. The aqueous layer was extracted with ethyl acetate (3×). The combined organics were dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The crude material was taken forward into the deprotection.

後処理

  1. customtransferred to a separatory funnel
  2. extractionThe aqueous layer was extracted with ethyl acetate (3×)
  3. dry with materialThe combined organics were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-78259ab45ee34577a6358ca68eecff2c
出典データセット
uspto-grants-2016_03
特許番号
US09273057B2

反応ノート

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