Acetone → HCID 21478689, 화합물

HRID 2292480노트

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HRID 2292480 반응식
[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:3]=1[OH:13].C([O-])([O-])=O.[K+].[K+].N[C@H](C(O)=O)[CH2:22][C:23]1[CH:32]=C2C(C=CC=C2)=C[CH:24]=1.CC(C)=O>CCCCCC>[CH:22]([O:13][C:3]1[C:4]([C:9]([CH3:10])([CH3:12])[CH3:11])=[CH:5][C:6]([Br:8])=[CH:7][C:2]=1[Br:1])=[C:23]([CH3:32])[CH3:24]

참가 물질

6

반응물 4

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 1859152-NaphthylalanineHCID 719757AKOS BBS-00008108

생성물 1

HCID 21478689HCID 21478689, 화합물

시약·촉매·용매 1

HCID 8058Hexane용매

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온도
23 °C

실험 절차

In a 3000 mL 3-neck flask, equipped with Ar inlet and magnetic stirrer, is placed 2,4-dibromo-6-tert-butylphenol (70.0 g, 226 mmol), K2CO3 (37.6 g, 276 mmol, 1.2 eq), Nal (3.38 g, 22.6 mmol, 0.1 eq), p-methallyl chloride (33.9 mL, 339 mmol, 1.5 eq), and acetone (1500 mL). The reaction mixture is vigorously stirred at 23° C. for 56 hrs, and monitored by TLC analysis (pet. ether). The solids are removed by filtration, washed with acetone, and the filtrates rotoevaporated (bath temperature kept below 35° C.) to give an oil. The oil is dissolved in hexane (100 mL), and stirred with silica gel (80 g). The slurry is filtered through a pad of Celite, and eluted with additional hexane (6×100 mL). The filtrate is evaporated to give 2,4-dibromo-6-tert-butylphenyl isobutenyl ether as a yellow oil. The material is stored in the freezer and is used as soon as possible.

후처리

  1. customIn a 3000 mL 3-neck flask, equipped with Ar inlet and magnetic stirrer
  2. customThe solids are removed by filtration
  3. washwashed with acetone
  4. custom(bath temperature kept below 35° C.)
  5. customto give an oil
  6. stirringstirred with silica gel (80 g)
  7. filtrationThe slurry is filtered through a pad of Celite
  8. washeluted with additional hexane (6×100 mL)
  9. customThe filtrate is evaporated

출처 및 근거

ORD 기록
ord-dfc69dbf69974418aa22863781b3c34d
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05684002

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