Potassium Carbonate → HCID 22179696、化合物

HRID 1796617ノート

反応式

HRID 1796617 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:6]([CH3:17])=[C:7]2[C:12](Cl)=[C:11]([C:14]#[N:15])[CH:10]=[N:9][N:8]2[CH:16]=1)=[O:4].[C:18]([O:22][C:23](=[O:42])[C:24]([O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=1[O:34][C:35]1[CH:40]=[CH:39][C:38]([NH2:41])=[CH:37][CH:36]=1)([CH3:26])[CH3:25])([CH3:21])([CH3:20])[CH3:19].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:1][O:2][C:3]([C:5]1[C:6]([CH3:17])=[C:7]2[C:12]([NH:41][C:38]3[CH:39]=[CH:40][C:35]([O:34][C:29]4[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=4[O:27][C:24]([C:23]([O:22][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:42])([CH3:26])[CH3:25])=[CH:36][CH:37]=3)=[C:11]([C:14]#[N:15])[CH:10]=[N:9][N:8]2[CH:16]=1)=[O:4]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 210251742-[2-(4-Amino-phenoxy)-phenoxy]-2-methyl-propionic acid tert-butyl esterHCID 69327667HCID 69327667、化合物

生成物 1

HCID 22179696HCID 22179696、化合物収率 91%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4-chloro-3-cyano-5-methyl-pyrrolo[1,2-b]pyridazine-6-carboxylic acid methyl ester (prepared using the procedure of Example 1D) (320 mg, 1.28 mmol), aniline 388C (440 mg, 1.28 mmol) and K2CO3 (1.77 g, 12.8 mmol) in anhydrous DMF (8 ml) was stirred at rt for 16 h. After regular workup, the residue was purified by silica gel flash column chromatography to afford 388D (651 mg, 91%) as a faintly yellow solid (0%-4% EtOAc—CH2Cl2). LCMS Found: (M+H)+=556.8; (M−tBu+2H)+=500.9

後処理

  1. customprepared
  2. customAfter regular workup, the residue was purified by silica gel flash column chromatography

出典と根拠

ORDレコード
ord-02cdab12942c4f53809d9bc0de5ef5a8
出典データセット
uspto-grants-2006_04
特許番号
US07030112B2

反応ノート

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