Ethoxalyl chloride → HCID 66880855, 화합물

HRID 1844534노트

반응식

HRID 1844534 반응식
Cl[C:2](=[O:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[Cl-].[Al+3].[Cl-].[Cl-].[CH3:13][O:14][CH2:15][CH2:16][S:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(Cl)Cl>[CH2:6]([O:5][C:3](=[O:4])[C:2]([C:21]1[CH:22]=[CH:23][C:18]([S:17][CH2:16][CH2:15][O:14][CH3:13])=[CH:19][CH:20]=1)=[O:8])[CH3:7]

참가 물질

5

반응물 3

HCID 20884Ethoxalyl chlorideHCID 40561742-METHOXYETHYL PHENYL SULFIDEHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 66880855HCID 66880855, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Ethyl chloroglyoxylate (8.76 mL) was added dropwise to a suspension of aluminum chloride (13.2 g, crushed) in methylene chloride (127 mL) under stirring and cooling with ice, and (2-methoxyethyl)phenylsulfide (12.0 g) was added dropwise thereto. The mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into ice water (200 mL), and the mixture was stirred for 10 minutes. The organic layer was separated, washed with a saturated aqueous sodium hydrogen carbonate solution (40 mL×3), and washed with saturated brine (60 mL). The washed organic layer was dried over anhydrous sodium sulfate, filtrated, and evaporated under reduced pressure. The obtained residue was purified by column chromatography (silica gel, hexane:ethyl acetate=4:1) to give 2-[4-(2-methoxyethylthio)phenyl]-2-oxoacetic acid ethyl ester (1.98 g).

후처리

  1. additionwas added dropwise
  2. stirringThe mixture was stirred at room temperature for 2 hours
  3. stirringthe mixture was stirred for 10 minutes
  4. customThe organic layer was separated
  5. washwashed with a saturated aqueous sodium hydrogen carbonate solution (40 mL×3)
  6. washwashed with saturated brine (60 mL)
  7. dry with materialThe washed organic layer was dried over anhydrous sodium sulfate
  8. filtrationfiltrated
  9. customevaporated under reduced pressure
  10. customThe obtained residue was purified by column chromatography (silica gel, hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-9a86842437eb420f9dabc433690f8d81
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946440B2

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