Water → HCID 86686014, 화합물

HRID 2277719노트

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HRID 2277719 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 6367Acetyl chlorideHCID 86686012HCID 86686012, 화합물

생성물 1

HCID 86686014HCID 86686014, 화합물수율 40%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-19e11730ccf9429885fb0711f3f3a664
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133158B2

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