Picolyl chloride hydrochloride → HCID 178418295、化合物

HRID 3236

反応式

HRID 3236 の反応式
[NH:1]1[CH2:7][C:5](=[O:6])[NH:4][C:2]1=[S:3].C[O-].[Na+].Cl.Cl[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1>CO>[N:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][S:3][C:2]1[NH:1][CH2:7][C:5](=[O:6])[N:4]=1

参加物

5

反応物 3

HCID 23392Picolyl chloride hydrochlorideHCID 12740302-ThiohydantoinHCID 10942334Sodium Methoxide

生成物 1

HCID 178418295HCID 178418295、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Initially, 1 g of 2-thiohydantoin and 2.5 g of sodium methylate were dissolved in 50 mL of methanol (MeoH), and 1.5 g of 2-chloromethylpyridine hydrochloride was added to the solution. The reaction mixture was stirred under reflux for one and a half hour and concentrated in vacuo. To the residue, there was added 50 mL of chloroform (CHCl3), and the mixture was washed with 50 mL of water. Then, the CHCL3 layer was dried over magnesium sulfate (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography [using a developing solvent consisting of CHCl3 :MeOH=50:1 (volume ratio, v/v)]. Recrystallization from diethylether gave the desired compound in the form of a needle-like crystal. The yield of this compound was 1.2 g with a yield ratio of 67.2%, and its melting point was 105°-107° C.

後処理

  1. temperatureunder reflux for one and a half hour
  2. concentrationconcentrated in vacuo
  3. additionTo the residue, there was added 50 mL of chloroform (CHCl3)
  4. washthe mixture was washed with 50 mL of water
  5. dry with materialThen, the CHCL3 layer was dried over magnesium sulfate (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography [
  8. customRecrystallization from diethylether

出典と根拠

ORDレコード
ord-ee329cf9c57341ee87f8398d0e4b9f66
出典データセット
uspto-grants-1998_03
特許番号
US05733922

関連ノート

読み込み中…