Water → HCID 86686014、化合物

HRID 2277719ノート

反応式

HRID 2277719 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[N:6]([C:12]1[CH:13]=[N:14][CH:15]=[C:16]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[CH:17]=1)[C:5]2([CH3:25])[CH3:24].[C:26](Cl)(=[O:28])[CH3:27].O>C(Cl)Cl>[C:26]([N:21]1[CH2:22][CH2:23][N:18]([C:16]2[CH:17]=[C:12]([N:6]3[C:5]([CH3:25])([CH3:24])[C:4]4[C:8](=[CH:9][CH:10]=[C:2]([Cl:1])[CH:3]=4)[C:7]3=[O:11])[CH:13]=[N:14][CH:15]=2)[CH2:19][CH2:20]1)(=[O:28])[CH3:27]

参加物

5

反応物 3

HCID 962WaterHCID 6367Acetyl chlorideHCID 86686012HCID 86686012、化合物

生成物 1

HCID 86686014HCID 86686014、化合物収率 40%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-chloro-3,3-dimethyl-2-(5-piperazin-1-yl-pyridin-3-yl)-2,3-dihydro-isoindol-1-one (52 mg, 0.146 mmol) and TEA (29.5 mg, 0.292 mmol) in DCM (5 mL) was added acetyl chloride (17.2 mg, 0.219 mmol) dropwise at 0° C. After stirring for 1 hour at room temperature, the mixture was treated with water and extracted with DCM. The organic layer was dried over anhy. Na2SO4. After removal of solvent, the residue was purified by preparative HPLC to afford the title compound as a white solid (23 mg, 40%). MS: 399.2 (M+H+).

後処理

  1. extractionextracted with DCM
  2. customThe organic layer was dried over anhy
  3. customAfter removal of solvent
  4. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-19e11730ccf9429885fb0711f3f3a664
出典データセット
uspto-grants-2015_09
特許番号
US09133158B2

反応ノート

読み込み中…