Triethylamine → HCID 89922461, 화합물

HRID 921917노트

반응식

HRID 921917 반응식
[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

참가 물질

7

반응물 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

생성물 1

HCID 89922461HCID 89922461, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-78259ab45ee34577a6358ca68eecff2c
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09273057B2

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