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Benzyltrimethylammonium hydroxide → HCID 370270, 화합물

HRID 2220681
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HRID 2220681 반응식
[C:1]1([CH3:18])[CH:6]=[CH:5][C:4]([CH2:7][C:8](=[O:17])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)=[CH:3][CH:2]=1.[CH3:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]([C:28]([C:30]2[CH:35]=[CH:34][C:33]([CH3:36])=[CH:32][CH:31]=2)=O)=O)=[CH:22][CH:21]=1.[OH-].C([N+](C)(C)C)C1C=CC=CC=1>C(O)C>[C:1]1([CH3:18])[CH:6]=[CH:5][C:4]([C:7]2[C:8](=[O:17])[C:9]([C:10]3[CH:11]=[CH:12][C:13]([CH3:16])=[CH:14][CH:15]=3)=[C:28]([C:30]3[CH:35]=[CH:34][C:33]([CH3:36])=[CH:32][CH:31]=3)[C:26]=2[C:23]2[CH:22]=[CH:21][C:20]([CH3:19])=[CH:25][CH:24]=2)=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 66854Benzyltrimethylammonium hydroxideHCID 769961,2-Bis(4-methylphenyl)-1,2-ethanedioneHCID 124202141,3-Bis(4-methylphenyl)propan-2-one

생성물 1

HCID 370270HCID 370270, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

23.13 g (0.11 mol) of 1,3-bis(p-tolyl)-2-propanone and 26.2 g (0.11 mol) of 4,4′-dimethylbenzil were dissolved in 75 ml of hot ethanol (abs.). 53 ml of a methanolic benzyltrimethylammonium hydroxide solution (0.11 mol Triton B, 35% Fluka) were slowly added dropwise at 80° C. with stirring (caution: the reaction batch froths vigorously) and refluxing was effected for 25 minutes. The crude product was filtered off after three hours, then washed with cold ethanol and recrystallized from toluene (violet red, yield: 46.2 g (95%); m.p.: 244-245° C., literature: 250.4-251.4° C. [15]; elemental analysis for C33H38O: found: C, 89.8%, H, 6.6%. calculated: C, 89.96%, H, 6.41%, MS-El [m/z (rel. intensity): M+440 (100), 412 (47), 206 (98), 191 (16), 189 (10)). The IR spectrum of 1,2,3,4-tetra(p-tolyl)cyclopenta-1,3-dien-5-one is shown in FIG. 10.

후처리

  1. temperaturethe reaction batch froths vigorously) and refluxing
  2. filtrationThe crude product was filtered off after three hours
  3. washwashed with cold ethanol
  4. customrecrystallized from toluene (violet red, yield: 46.2 g (95%)
  5. custom250.4-251.4° C. [15]

출처 및 근거

ORD 기록
ord-31efafc87f324f3991366b5227a41a6d
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07417247B2

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