Potassium Carbonate → HCID 86761923、化合物

HRID 448568

反応式

HRID 448568 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:17]1[N:22]=[CH:21][N:20]=[C:19]([N:23]2[C:31]3[C:26](=[CH:27][C:28]([S:32]([CH3:35])(=[O:34])=[O:33])=[CH:29][CH:30]=3)[CH2:25][CH2:24]2)[CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>CC(N(C)C)=O.C(Cl)Cl.[Cl-].[Na+].O>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([C:17]2[CH:18]=[C:19]([N:23]3[C:31]4[C:26](=[CH:27][C:28]([S:32]([CH3:35])(=[O:33])=[O:34])=[CH:29][CH:30]=4)[CH2:25][CH2:24]3)[N:20]=[CH:21][N:22]=2)[CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 41361281-benzyl-N-methylpiperidin-4-amineHCID 595665261-(6-Chloropyrimidin-4-yl)-5-(methylsulfonyl)indoline

生成物 1

HCID 86761923HCID 86761923、化合物

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 31374Dimethylacetamide溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 7b (0.14 g, 2.1 eq), 6a (0.1 g, 0.3 mmol) and potassium carbonate (0.1 g, 2.2 eq) in 1 mL of DMA was heated up to 90° C. for 48 h then cooled down to room temperature and diluted with DCM (2 mL) and brine (2 mL). The layers were separated and the aqueous extracted with DCM (2×2 mL). The combined extracts were washed with brine (2×50 mL), dried over magnesium sulfate, filtered and evaporated. The residue was diluted with acetonitrile and purified on preparative HPLC to afford 7c.

後処理

  1. temperaturethen cooled down to room temperature
  2. customThe layers were separated
  3. extractionthe aqueous extracted with DCM (2×2 mL)
  4. washThe combined extracts were washed with brine (2×50 mL)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. additionThe residue was diluted with acetonitrile
  9. custompurified on preparative HPLC

出典と根拠

ORDレコード
ord-94807e5ba900447ca162d4865b48c8e6
出典データセット
uspto-grants-2013_07
特許番号
US08481731B2

関連ノート

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