Thionyl Chloride → Ethyl 6-chloromethyl-2-oxo-2H-1-benzopyran-3-carboxylate

HRID 276973노트

반응식

HRID 276973 반응식
O[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][C:10](=[O:12])[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8][C:7]=2[CH:18]=1.S(Cl)([Cl:21])=O>C(Cl)(Cl)Cl>[Cl:21][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][C:10](=[O:12])[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8][C:7]=2[CH:18]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 10586607HCID 10586607, 화합물

생성물 1

HCID 10659438Ethyl 6-chloromethyl-2-oxo-2H-1-benzopyran-3-carboxylate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 1 g of ethyl 6-hydroxymethyl-2-oxo-2H-1-benzopyran-3-carboxylate (3.9 mmol) and 10 ml of thionyl chloride is refluxed for 3 h. The solution obtained is evaporated under reduced pressure. The residue is re-suspended in 10 ml of dry toluene and the solvent is evaporated off under reduced pressure. The last two steps are repeated twice. The residue obtained is taken up in chloroform and the organic phase is washed three times with 0.1 N HCl solution and then dried over MgSO4. The solvent is removed by distillation under reduced pressure and the residue is recrystallized from CHCl3/Petroleum ether.

후처리

  1. temperatureis refluxed for 3 h
  2. customThe solution obtained
  3. customis evaporated under reduced pressure
  4. customthe solvent is evaporated off under reduced pressure
  5. customThe residue obtained
  6. washthe organic phase is washed three times with 0.1 N HCl solution
  7. dry with materialdried over MgSO4
  8. customThe solvent is removed by distillation under reduced pressure
  9. customthe residue is recrystallized from CHCl3/Petroleum ether

출처 및 근거

ORD 기록
ord-438769c7c6c2448bbf0cb3ef65cd0d6f
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355658B1

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