Acetohydroxamic Acid → HCID 68478268、化合物

HRID 2239882ノート

反応式

HRID 2239882 の反応式
C([NH:4][OH:5])(=O)C.CC(C)([O-])C.[K+].C1COCC1.F[C:18]1[CH:25]=[CH:24][C:23]([C:26]2[CH:27]=[C:28]([N:35]([CH2:42][C:43]3[CH:48]=[CH:47][C:46]([O:49][CH3:50])=[CH:45][CH:44]=3)[C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[C:29]3[N:30]([CH:32]=[CH:33][N:34]=3)[N:31]=2)=[CH:22][C:19]=1[C:20]#[N:21]>CN(C=O)C.CO>[CH3:50][O:49][C:46]1[CH:45]=[CH:44][C:43]([CH2:42][N:35]([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[C:28]2[C:29]3[N:30]([CH:32]=[CH:33][N:34]=3)[N:31]=[C:26]([C:23]3[CH:24]=[CH:25][C:18]4[O:5][N:4]=[C:20]([NH2:21])[C:19]=4[CH:22]=3)[CH:27]=2)=[CH:48][CH:47]=1

参加物

7

反応物 4

HCID 1990Acetohydroxamic AcidHCID 8028TetrahydrofuranHCID 23665647Potassium tert-butoxideHCID 684836932-Fluoro-5-(8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazin-6-yl)benzonitrile

生成物 1

HCID 68478268HCID 68478268、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of acetohydroxamic acid (42 mg, 0.556 mmol) in DMF (1 mL) was added a solution of potassium t-butoxide in THF (0.56 mL, 0.56 mmol). The reaction solution was stirred at RT for 15 minutes and then a solution of 2-fluoro-5-(8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazin-6-yl)benzonitrile (25 mg, 0.056 mmol) from (1b) in DMF (1 mL) was added. The reaction solution was stirred at RT for 24 hours. The solution was diluted with methanol and purified by preparative HPLC to give 5-(8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazin-6-yl)benzo[d]isoxazol-3-amine. LC/MS, m/e 463 (M+1). HPLC Rt, 3.13 min. Waters Sunfire C18 column (4.6×50 mm). 0%-100% B. Solvent B: (90% MeOH, 10% H2O, 0.1% TFA). Solvent A: (10% MeOH, 90% H2O, 0.1% TFA). Gradient, start % B=0, final % B=100, gradient time 4 min. hold at 100% B 1 min, flow rate 4 mL/min.

後処理

  1. stirringThe reaction solution was stirred at RT for 24 hours
  2. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-02d753a69abc410db4201d46f37368fb
出典データセット
uspto-grants-2010_05
特許番号
US07723336B2

反応ノート

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