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Benzyltrimethylammonium hydroxide → HCID 370270、化合物

HRID 2220681
ノート
印刷プレビュー

反応式

HRID 2220681 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 370270HCID 370270、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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]

出典と根拠

ORDレコード
ord-31efafc87f324f3991366b5227a41a6d
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07417247B2

反応ノート

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