Methanol → HCID 15321723, 화합물

HRID 1914411노트

반응식

HRID 1914411 반응식
[C:1]([C:5]1[CH:6]=[C:7]2[C:19]3=[C:20]4[C:10](=[CH:11][CH:12]=[C:13]([CH3:21])[C:14]4=[CH:15][CH:16]=[C:17]3[CH:18]=1)[CH:9]=[CH:8]2)([CH3:4])([CH3:3])[CH3:2].CO.[Br-:24].[Br-].[Br-].C([N+](C)(C)C)C1C=CC=CC=1.C([N+](C)(C)C)C1C=CC=CC=1.C([N+](C)(C)C)C1C=CC=CC=1.O>ClCCl>[Br:24][C:11]1[C:10]2[C:20]3=[C:19]4[C:7](=[CH:8][CH:9]=2)[CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:18]=[C:17]4[CH:16]=[CH:15][C:14]3=[C:13]([CH3:21])[CH:12]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 30866837-tert-Butyl-1-methylpyreneHCID 53442637Benzyltrimethylammoniumtribromide

생성물 1

HCID 15321723HCID 15321723, 화합물수율 155.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Next, a mixed solution of 3 g of 7-t-butyl-1-methylpyrene, 130 ml of dichloromethane and 43 ml of methanol was cooled to 0° C. under a nitrogen gas stream and then 4.3 g of benzyltrimethylammonium tribromide dissolved in 5 ml of dichloromethane was added dropwise. This mixed solution was stirred at room temperature for 4 hours and 50 ml of water was poured into the solution, followed by extraction with 50 ml of dichloromethane. The organic layer was washed twice with 50 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 3.4 g of 1-bromo-7-t-butyl-3-methylpyrene.

후처리

  1. additionwas added dropwise
  2. extractionfollowed by extraction with 50 ml of dichloromethane
  3. washThe organic layer was washed twice with 50 ml of water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customThe concentrate was purified by silica gel column chromatography
  7. customvacuum-dried

출처 및 근거

ORD 기록
ord-de25a688f34444eb87a789c9a8ae07b5
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08610345B2

반응 노트

불러오는 중…