N,N'-二环己基碳二亚胺 → 3-({4-[3-(3,4-Dimethoxyphenyl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}carbonyl)phenyl acetate

HRID 524145

反应方程式

HRID 524145 反应方程式
Cl.[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:12]2[C:13]([CH3:25])([CH3:24])[C:14](=[O:23])[N:15]([CH:17]3[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)[N:16]=2)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11].[C:26]([O:29][C:30]1[CH:31]=[C:32]([CH:36]=[CH:37][CH:38]=1)[C:33](O)=[O:34])(=[O:28])[CH3:27].C1CCC(N=C=NC2CCCCC2)CC1>C(Cl)Cl>[C:26]([O:29][C:30]1[CH:38]=[CH:37][CH:36]=[C:32]([C:33]([N:20]2[CH2:21][CH2:22][CH:17]([N:15]3[C:14](=[O:23])[C:13]([CH3:25])([CH3:24])[C:12]([C:6]4[CH:7]=[CH:8][C:9]([O:10][CH3:11])=[C:4]([O:3][CH3:2])[CH:5]=4)=[N:16]3)[CH2:18][CH2:19]2)=[O:34])[CH:31]=1)(=[O:28])[CH3:27]

参与物

5

反应物 3

HCID 10868N,N'-二环己基碳二亚胺HCID 238669间乙酰苯甲酸HCID 666164065-(3,4-dimethoxyphenyl)-4,4-dimethyl-2-piperidin-4-yl-2,4-dihydro-3H-pyrazol-3-one hydrochloride2 次

产物 1

HCID 462027213-({4-[3-(3,4-Dimethoxyphenyl)-4,4-dimethyl-5-oxo-4,5-dihydro-1H-pyrazol-1-yl]piperidin-1-yl}carbonyl)phenyl acetate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

A mixture of 10 g 5-(3,4-dimethoxyphenyl)-4,4-dimethyl-2-(piperidin-4-yl)-2,4-dihydro-3H-pyrazol-3-one (compound B1), 8 g of 3-(acetyloxy)benzoic acid and 7 g of DCC in 150 ml of DCM is stirred for 2 h until the reaction is complete according to TLC analysis. The reaction mixture is quenched with water, the phases are separated and the organic phase is washed with water again. The organic phase is dried over MgSO4, and the solvent is removed under reduced pressure resulting in a crude product, which is purified by crystallization from methanol to yield the title compound.

后处理

  1. customThe reaction mixture is quenched with water
  2. customthe phases are separated
  3. washthe organic phase is washed with water again
  4. dry with materialThe organic phase is dried over MgSO4
  5. customthe solvent is removed under reduced pressure
  6. customresulting in a crude product, which
  7. customis purified by crystallization from methanol

来源与证据

ORD记录
ord-00e8849f8046435882f0a5e8979fbacf
来源数据集
uspto-grants-2016_05
专利号
US09340522B2

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