Potassium Carbonate → HCID 59401321、化合物

HRID 2060894ノート

反応式

HRID 2060894 の反応式
Cl[C:2]1[C:11]2[C:6](=[C:7]([CH2:12][NH2:13])[CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].[OH:20][C:21]1[CH:29]=[CH:28][C:24]([C:25]([NH2:27])=[O:26])=[CH:23][CH:22]=1>CN(C=O)C>[NH2:13][CH2:12][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:6]=1[N:5]=[CH:4][CH:3]=[C:2]2[O:20][C:21]1[CH:29]=[CH:28][C:24]([C:25]([NH2:27])=[O:26])=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 650524-HydroxybenzamideHCID 59401376HCID 59401376、化合物

生成物 1

HCID 59401321HCID 59401321、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of C-(4-chloroquinolin-8-yl)methylamine (Preparation 89) (129 mg, 0.67 mmol), K2CO3 (186 mg, 1.34 mmol) and 4-hydroxybenzamide (110 mg, 0.81 mmol) in DMF (4 mL) were heated in a microwave at 100° C. for 40 min (150 W). Solvent removed in vacuo. The mixture was partitioned between EtOAc (50 mL) and water (20 mL), and the aqueous phase was further extracted with EtOAc (2×20 mL). The combined organic phase was washed with brine (20 mL) and dried (MgSO4). Solvent was removed in vacuo and the residue purified by column chromatography (0.25% to 0.75% NH4OH(aq), 2% to 8% MeOH in DCM) to give the title compound: RT=2.15 min; m/z (ES+)=294.1 [M+H]+.

後処理

  1. customSolvent removed in vacuo
  2. customThe mixture was partitioned between EtOAc (50 mL) and water (20 mL)
  3. extractionthe aqueous phase was further extracted with EtOAc (2×20 mL)
  4. washThe combined organic phase was washed with brine (20 mL)
  5. dry with materialdried (MgSO4)
  6. customSolvent was removed in vacuo
  7. customthe residue purified by column chromatography (0.25% to 0.75% NH4OH(aq), 2% to 8% MeOH in DCM)

出典と根拠

ORDレコード
ord-a342471fe9354d15864dcab686197e36
出典データセット
uspto-grants-2012_10
特許番号
US08278442B2

反応ノート

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