Acetyl chloride → 4-(n-Acetyl-cyclopentylamino)-3-methyl-iodobenzene

HRID 891967ノート

反応式

HRID 891967 の反応式
[CH:1]1([NH:6][C:7]2[CH:12]=[CH:11][C:10]([I:13])=[CH:9][C:8]=2[CH3:14])[CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].[C:17](Cl)(=[O:19])[CH3:18]>O1CCCC1>[C:17]([N:6]([CH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1)[C:7]1[CH:12]=[CH:11][C:10]([I:13])=[CH:9][C:8]=1[CH3:14])(=[O:19])[CH3:18]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 24758Sodium hydrideHCID 222410484-Cyclopentylamino-3-methyl-iodobenzene

生成物 1

HCID 111752944-(n-Acetyl-cyclopentylamino)-3-methyl-iodobenzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

0.5 g (1.7 mmol) of 4-cyclopentylamino-3-methyl-iodobenzene are dissolved in 20 ml tetrahydrofuran and after the addition of 81.3 mg (1.7 mmol) of sodium hydride (50% in oil) stirred for 1 hour at 40 ° C. After cooling to ambient temperature 0.1 ml (1.5 mmol) of acetyl chloride is added and the mixture is stirred overnight at ambient temperature. The solvent is distilled off and the residue distributed in water/ethyl acetate. The combined organic extracts are dried, concentrated by evaporation and chromatographed on silica gel, eluting with dichloromethane/ethanol 0 to 5%.

後処理

  1. additionis added
  2. stirringthe mixture is stirred overnight at ambient temperature
  3. distillationThe solvent is distilled off
  4. customThe combined organic extracts are dried
  5. concentrationconcentrated by evaporation
  6. customchromatographed on silica gel
  7. washeluting with dichloromethane/ethanol 0 to 5%

出典と根拠

ORDレコード
ord-3e84509824ca4332bb6b82f653a5e3a5
出典データセット
uspto-grants-2006_02
特許番号
US07005437B2

反応ノート

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