1-Methylpiperazine → HCID 21854014、化合物

HRID 254190ノート

反応式

HRID 254190 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]([OH:12])=O)=[CH:2]1.C(Cl)(=O)C(Cl)=O.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>ClCCl>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]([N:23]2[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]2)=[O:12])=[CH:2]1

参加物

5

反応物 3

HCID 531671-MethylpiperazineHCID 65578Oxalyl chlorideHCID 69867Indole-3-Carboxylic Acid

生成物 1

HCID 21854014HCID 21854014、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

1H-Indole-3-carboxylic acid (1.61 g, 0.01 moles) was stirred with oxalyl chloride (0.99 g, 0.011 moles) in 20 mL dichloromethane at 0 to 25° C. for 3-4 hours. After completion of the reaction (TLC), volatile substances were distilled off under the reduced pressure. The residue was taken in 20 mL dichloroethane and to this stirred solution, was added N-methylpiperazine (1.1 g, 0.011 moles). The reaction mixture was further stirred for next 3-5 hours, till the reaction completes (TLC). Reaction mixture was diluted with dichloromethane 20 mL), washed with water, brine and saturated solution of sodium bicarbonate. The organic layer was dried over sodium sulfate and the organic solvents were evaporated under vacuo. The product was purified using column chromatography on silica gel G stationary phase and suitable combinations of ethyl acetate and methanol in increasing gradient, as the mobile phase.

後処理

  1. customAfter completion of the reaction (TLC), volatile substances
  2. distillationwere distilled off under the reduced pressure
  3. customReaction mixture
  4. washwashed with water, brine and saturated solution of sodium bicarbonate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. customthe organic solvents were evaporated under vacuo
  7. customThe product was purified
  8. temperaturein increasing gradient

出典と根拠

ORDレコード
ord-cc4e0ab2ff76430bafd695424be4e25e
出典データセット
uspto-grants-2011_01
特許番号
US07875605B2

反応ノート

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