碳酸钾 → 4-[6-(5-Methanesulfonyl-2,3-dihydro-indol-1-yl)-pyrimidin-4-ylamino]-piperidine-1-carboxylic acid tert-butyl ester

HRID 448564

反应方程式

HRID 448564 反应方程式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([N:8]2[C:16]3[C:11](=[CH:12][C:13]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:14][CH:15]=3)[CH2:10][CH2:9]2)[CH:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][CH:31]([NH2:34])[CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22].CC(N(C)C)=O.C(=O)([O-])[O-].[K+].[K+]>[Cl-].[Na+].O>[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][CH:31]([NH:34][C:2]2[CH:3]=[C:4]([N:8]3[C:16]4[C:11](=[CH:12][C:13]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:14][CH:15]=4)[CH2:10][CH2:9]3)[N:5]=[CH:6][N:7]=2)[CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

参与物

6

反应物 4

HCID 11430碳酸钾HCID 31374N,N-二甲基乙酰胺HCID 12682911-Boc-4-氨基哌啶HCID 595665261-(6-Chloropyrimidin-4-yl)-5-(methylsulfonyl)indoline

产物 1

HCID 580741254-[6-(5-Methanesulfonyl-2,3-dihydro-indol-1-yl)-pyrimidin-4-ylamino]-piperidine-1-carboxylic acid tert-butyl ester

试剂、催化剂与溶剂 1

HCID 57417360Sodium chloride; water溶剂

反应条件

温度
80 °C

实验过程

A mixture of 6a (0.4 g, 1.29 mmol), 4-amino-piperidine-1-carboxylic acid tert-butyl ester (0.4 g, 1.5 eq), DMA (5 mL) and potassium carbonate (0.4 g, 2.2 eq) was heated at 80° C. for 42 h. After allowing the reaction mixture to cool down to room temperature, 100 mL of brine was added and the mixture was extracted with ethyl acetate twice (100 mL and 30 mL). The combined extracts were washed with brine (2×50 mL), dried over magnesium sulfate and filtered. The solvent was removed under vacuum to give a solution of 6b in DMA.

后处理

  1. temperatureto cool down to room temperature
  2. extractionthe mixture was extracted with ethyl acetate twice (100 mL and 30 mL)
  3. washThe combined extracts were washed with brine (2×50 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customThe solvent was removed under vacuum

来源与证据

ORD记录
ord-4a1b421ad8224d65bd9a3b41614f8ef6
来源数据集
uspto-grants-2013_07
专利号
US08481731B2

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