Sodium hydride → HCID 131730788、化合物

HRID 80944

反応式

HRID 80944 の反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:15]=[N:14][C:13]([C:16]3[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=3)=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[H-].[Na+].[Cl:25][CH2:26][C:27]([N:29]([CH3:31])[CH3:30])=[O:28]>CN(C=O)C>[ClH:25].[ClH:25].[CH:1]([N:4]1[CH2:5][CH2:6][N:7]([C:10]2[N:15]=[N:14][C:13]([C:16]3[CH:17]=[CH:18][C:19]([O:22][CH2:26][C:27]([N:29]([CH3:31])[CH3:30])=[O:28])=[CH:20][CH:21]=3)=[CH:12][CH:11]=2)[CH2:8][CH2:9]1)([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 758862-chloro-N,N-dimethylacetamideHCID 1360994094-(6-(4-Isopropylpiperazin-1-yl)-pyridazin-3-yl)-phenol

生成物 1

HCID 131730788HCID 131730788、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A mixture of 4-[6-(4-isopropyl-piperazin-1-yl)-pyridazin-3-yl]-phenol (110 mg, 0.37 mmol) and 60% sodium hydride (58 mg, 1.45 mmol) in dry DMF (5 mL) was heated at 60° C. for 30 min. 2-Chloro-N,N-dimethylacetamide (54 mg, 0.44 mmol) was added and heating at 60° C. was continued for another 20 h. The reaction mixture was evaporated to dryness and partitioned between water (10 mL) and DCM (10 mL). The organic phase was isolated, washed with brine (5 mL), dried over anhydrous magnesium sulphate, and evaporated to dryness in vacuo. The residue was dissolved in hot ethyl acetate and HClg in Et2O was added to give the title compound.

後処理

  1. temperatureheating at 60° C.
  2. customThe reaction mixture was evaporated to dryness
  3. custompartitioned between water (10 mL) and DCM (10 mL)
  4. customThe organic phase was isolated
  5. washwashed with brine (5 mL)
  6. dry with materialdried over anhydrous magnesium sulphate
  7. customevaporated to dryness in vacuo
  8. dissolutionThe residue was dissolved in hot ethyl acetate
  9. additionHClg in Et2O was added

出典と根拠

ORDレコード
ord-ad58286448e340c4add39b118395f36f
出典データセット
uspto-grants-2014_09
特許番号
US08846677B2

関連ノート

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