Picolyl chloride hydrochloride → HCID 178418295, 화합물

HRID 3236

반응식

HRID 3236 반응식
[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

참가 물질

5

반응물 3

HCID 23392Picolyl chloride hydrochlorideHCID 12740302-ThiohydantoinHCID 10942334Sodium Methoxide

생성물 1

HCID 178418295HCID 178418295, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ee329cf9c57341ee87f8398d0e4b9f66
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733922

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