Dimethyl Sulfoxide → HCID 67098970、化合物

HRID 2077091ノート

反応式

HRID 2077091 の反応式
[Cl:1][C:2]1[N:9]=[C:8]([NH:10][C:11]2[CH:15]=[C:14]([CH3:16])[NH:13][N:12]=2)[CH:7]=[C:6]([CH3:17])[C:3]=1[C:4]#[N:5].[Cl:18][C:19]1[CH:28]=[CH:27][CH:26]=[CH:25][C:20]=1[O:21][CH2:22][CH2:23][NH2:24].C(=O)([O-])O.[Na+].CS(C)=O>O>[ClH:1].[Cl:18][C:19]1[CH:28]=[CH:27][CH:26]=[CH:25][C:20]=1[O:21][CH2:22][CH2:23][NH:24][C:2]1[N:9]=[C:8]([NH:10][C:11]2[CH:15]=[C:14]([CH3:16])[NH:13][N:12]=2)[CH:7]=[C:6]([CH3:17])[C:3]=1[C:4]#[N:5]

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 516892Sodium BicarbonateHCID 27357882-(2-Chlorophenoxy)EthylamineHCID 119835452-chloro-6-(5-methyl-1H-pyrazol-3-ylamino)-4-methylnicotinonitrile

生成物 1

HCID 67098970HCID 67098970、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

Compound A (200 mg, 813 μmol), 2-(2-chlorophenoxy)ethylamine (280 μl) and sodium hydrogencarbonate (683 mg) were added to DMSO (6 ml), and the mixture was stirred at 100° C. for 27 hr. After stirring, the reaction mixture was added to cold water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and concentrated, and the residue was washed by suspending in ethyl acetate. This was converted to hydrochloride to give the object compound of 2-(2-(2-chlorophenoxy)ethylamino)-6-(5-methyl-1H-pyrazol-3-ylamino)-4-methylnicotinonitrile hydrochloride (18 mg).

後処理

  1. stirringAfter stirring
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. concentrationconcentrated
  5. washthe residue was washed

出典と根拠

ORDレコード
ord-ebbdc95c02e143f894b3d149257e4733
出典データセット
uspto-grants-2011_04
特許番号
US07928126B2

反応ノート

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