Dichloromethane → 7-tert-Butyl-1-methylpyrene

HRID 1914410노트

반응식

HRID 1914410 반응식
[CH3:1][C:2]1[C:15]2[C:16]3=[C:17]4[C:12](=[CH:13][CH:14]=2)[CH:11]=[CH:10][CH:9]=[C:8]4[CH:7]=[CH:6][C:5]3=[CH:4][CH:3]=1.[C:18](Cl)([CH3:21])([CH3:20])[CH3:19].ClCCl.[Cl-].[Al+3].[Cl-].[Cl-]>O>[C:18]([C:10]1[CH:9]=[C:8]2[C:17]3=[C:16]4[C:5](=[CH:4][CH:3]=[C:2]([CH3:1])[C:15]4=[CH:14][CH:13]=[C:12]3[CH:11]=1)[CH:6]=[CH:7]2)([CH3:21])([CH3:20])[CH3:19]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 10486tert-BUTYL CHLORIDEHCID 169321-MethylpyreneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 30866837-tert-Butyl-1-methylpyrene수율 54.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Next, a mixed solution of 4.4 g of 1-methylpyrene, 2 g of t-butylchloride and 33 ml of dichloromethane was cooled to 0° C. under a nitrogen gas stream and then 2.7 g of aluminum chloride was added. This mixed solution was stirred at room temperature for 3 hours and 30 ml of water was poured into the solution, followed by extraction with 30 ml of dichloromethane. The organic layer was washed twice with 20 ml of water, dried over magnesium sulfate and then evaporated. The concentrate was purified by silica gel column chromatography and then vacuum-dried to obtain 3 g of 7-t-butyl-1-methylpyrene.

후처리

  1. extractionfollowed by extraction with 30 ml of dichloromethane
  2. washThe organic layer was washed twice with 20 ml of water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customThe concentrate was purified by silica gel column chromatography
  6. customvacuum-dried

출처 및 근거

ORD 기록
ord-ae6368f67b7047a489bc72fcffdf2610
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08610345B2

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