Phenylacetyl chloride → HCID 10709050, 화합물

HRID 235192노트

반응식

HRID 235192 반응식
[C:1]1([CH2:7][CH2:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Al+3].[Cl-].[Cl-].[C:18]1([CH2:24][C:25](Cl)=[O:26])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(=S)=S>[C:18]1([CH2:24][C:25]([C:4]2[CH:5]=[CH:6][C:1]([CH2:7][CH2:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[CH:2][CH:3]=2)=[O:26])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 7679Phenylacetyl chlorideHCID 281254Methyl 4-phenylbutyrateHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 10709050HCID 10709050, 화합물수율 65.7%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매2회

실험 절차

To a solution of 25.0 g of methyl 4-phenylbutyrate in 100 ml of carbon disulfide, 37.3 g of anhydrous aluminium chloride was added and then a solution of 43.3 g of phenylacetyl chloride in 25 ml of carbon disulfide was added dropwise, and the mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into ice-water and extracted with methylene chloride. The methylene chloride layer was washed with aqueous potassium carbonate solution, dried, and then the solvent was removed. The residue was purified by column chromatography on silica gel (methylene chloride:n-hexane=2:1→methylene chloride) to afford 27.3 g of colorless crystals. Recrystallization from isopropyl ether gave colorless flakes, mp 54°~54.5° C.

후처리

  1. extractionextracted with methylene chloride
  2. washThe methylene chloride layer was washed with aqueous potassium carbonate solution
  3. customdried
  4. customthe solvent was removed
  5. customThe residue was purified by column chromatography on silica gel (methylene chloride:n-hexane=2:1→methylene chloride)

출처 및 근거

ORD 기록
ord-ffc49b6b7fb547d1ad87a90d1b605821
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05597848

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