Thioacetamide → HCID 66673711、化合物

HRID 421835ノート

反応式

HRID 421835 の反応式
[C:1]([NH2:4])(=[S:3])[CH3:2].Br[CH2:6][C:7]([N:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]1)=O>C(O)C>[CH3:2][C:1]1[S:3][CH:6]=[C:7]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[N:4]=1

参加物

4

反応物 2

HCID 2723949ThioacetamideHCID 15829155tert-Butyl 4-(bromoacetyl)piperazine-1-carboxylate

生成物 1

HCID 66673711HCID 66673711、化合物収率 2.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Thioacetamide (120 mg) was added to an ethanol (6 mL) solution of tert-butyl 4-(bromoacetyl)piperazinecarboxylate (340 mg) obtained in the above 1), and heated under reflux for 3 hours. The reaction liquid was restored to room temperature, then the solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=7/3) to obtain 7 mg of the entitled compound.

後処理

  1. customobtained in the above 1), and
  2. temperatureheated
  3. temperatureunder reflux for 3 hours
  4. customThe reaction liquid
  5. customwas restored to room temperature
  6. customthe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=7/3)

出典と根拠

ORDレコード
ord-5049bb1cc5e24c538645131813f4771e
出典データセット
uspto-grants-2012_01
特許番号
US08101618B2

反応ノート

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