Methanol → HCID 15321723、化合物

HRID 1914411ノート

反応式

HRID 1914411 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 15321723HCID 15321723、化合物収率 155.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-de25a688f34444eb87a789c9a8ae07b5
出典データセット
uspto-grants-2013_12
特許番号
US08610345B2

反応ノート

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