Thionyl Chloride → 2-Chloromethyl-4-(4-methoxybutoxy)pyridine

HRID 357569노트

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HRID 357569 반응식
O[CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH3:15])[CH:6]=[CH:5][N:4]=1.S(Cl)([Cl:18])=O.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[Cl:18][CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH3:15])[CH:6]=[CH:5][N:4]=1

참가 물질

5

반응물 3

HCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 151662242-Hydroxymethyl-4-(4-methoxybutoxy)pyridine

생성물 1

HCID 151662232-Chloromethyl-4-(4-methoxybutoxy)pyridine수율 83.6%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

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온도
0 °C

실험 절차

5.6 g of crude 2-hydroxymethyl-4-(4-methoxybutoxy)pyridine was dissolved in 80 ml of chloroform to obtain a solution. A solution of 3.8 g of thionyl chloride in 10 ml of chloroform was dropwise added to this solution at 0° C. The obtained mixture was stirred at 0° C. for one hour. After the completion of the reaction, the reaction mixture was neutralized with a saturated aqueous solution of sodium hydrogencarbonate and extracted with 200 ml of chloroform twice. The extract was dried over magnesium sulfate and filtered, The filtrate was distilled to remove the solvent. The obtained residue was dried in a vacuum to obtain 5.09 g of the title compound as a crude oil.

후처리

  1. customto obtain a solution
  2. customAfter the completion of the reaction
  3. extractionextracted with 200 ml of chloroform twice
  4. dry with materialThe extract was dried over magnesium sulfate
  5. filtrationfiltered
  6. distillationThe filtrate was distilled
  7. customto remove the solvent
  8. customThe obtained residue was dried in a vacuum

출처 및 근거

ORD 기록
ord-08491fda85c84c1c80e3dbc04e623d66
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840910

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