Dimethylformamide → 1-Bromo-3,6,8-tri(4-methylphenyl)pyrene

HRID 1027320노트

반응식

HRID 1027320 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:21]3[C:22]4=[C:23]5[C:18](=[CH:19][CH:20]=3)[CH:17]=[CH:16][C:15]([C:24]3[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=3)=[C:14]5[CH:13]=[CH:12][C:11]4=[C:10]([C:31]3[CH:36]=[CH:35][C:34]([CH3:37])=[CH:33][CH:32]=3)[CH:9]=2)=[CH:4][CH:3]=1.[Br:38]N1C(=O)CCC1=O.CN(C)C=O>O>[Br:38][C:17]1[C:18]2[C:23]3=[C:22]4[C:21](=[CH:20][CH:19]=2)[C:8]([C:5]2[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=2)=[CH:9][C:10]([C:31]2[CH:36]=[CH:35][C:34]([CH3:37])=[CH:33][CH:32]=2)=[C:11]4[CH:12]=[CH:13][C:14]3=[C:15]([C:24]2[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=2)[CH:16]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 67184N-bromobutanimideHCID 866285911,3,6-Tri(4-methylphenyl)pyrene

생성물 1

HCID 866285921-Bromo-3,6,8-tri(4-methylphenyl)pyrene수율 85.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Next, a mixed solution of 1.5 g of 1,3,6-tri(4-methylphenyl)pyrene, 0.68 g of N-bromosuccinimide and 30 ml of dimethylformamide was stirred under a nitrogen gas flow at 60° C. for 6 hours. After cooling to room temperature, 50 ml of water was injected, followed by extraction with 100 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate and then evaporated. The resultant concentrate was purified by silica gel column chromatography and then vacuum-dried to obtain 1.5 g of 1-bromo-3,6,8-tri(4-methylphenyl)pyrene as a pale yellow powder.

후처리

  1. extractionfollowed by extraction with 100 ml of dichloromethane
  2. washThe organic layer was washed twice with 50 ml of water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. concentrationThe resultant concentrate
  6. customwas purified by silica gel column chromatography
  7. customvacuum-dried

출처 및 근거

ORD 기록
ord-b353cb3c5dad469cb475ed4782b41790
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08729530B2

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