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Hydrochloric Acid → HCID 67285452、化合物

HRID 1943535
ノート
印刷プレビュー

反応式

HRID 1943535 の反応式
[C:1](Cl)(=[O:4])[CH:2]=[CH2:3].[OH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([C:19]3[CH:24]=[CH:23][C:22]([OH:25])=[CH:21][CH:20]=3)[CH:14]=2)=[CH:9][CH:8]=1.C(N([CH2:31][CH3:32])CC)C.Cl.[OH-:34].[Na+].Cl[CH2:37]Cl>C(C1C(O)=C(C(C)(C)C)C=C(C)C=1)(C)(C)C.O>[C:37]([O:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([C:19]3[CH:24]=[CH:23][C:22]([O:25][C:1](=[O:4])[CH:2]=[CH2:3])=[CH:21][CH:20]=3)[CH:14]=2)=[CH:11][CH:12]=1)(=[O:34])[CH:31]=[CH2:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 14798Sodium HydroxideHCID 667696[1,1':3',1''-Terphenyl]-4,4''-diol

生成物 1

HCID 67285452HCID 67285452、化合物

試薬・触媒・溶媒 2

HCID 314042,6-Di-tert-butyl-4-methylphenol触媒HCID 962Water溶媒2 回

実験手順

Acryloyl chloride (8.97 g, 99.1 mmol) was added dropwise to a mixture of dichloromethane (100 mL), the compound (T-8) (10.0 g, 38.1 mmol), triethylamine (10.0 g, 99.1 mmol) and 2,6-di-tert-butyl-p-cresol (8.4 mg, 0.0381 mmol) in an ice bath under an atmosphere of nitrogen, and then the mixture was warmed slowly to room temperature. The stirring was continued at room temperature for 16 hours, and the reaction mixture was poured into water. The organic layer was wished with 1M-hydrochloric acid, aqueous 1M-sodium hydroxide solution and water. After the organic layer had been dried over anhydrous magnesium sulfate, the organic solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: toluene), and then by recrystallization from a mixed solvent of ethanol and ethyl acetate to give colorless crystals (4.73 g) of 4,4″-bis(acryloyloxy)-(1,1′:3′,1″)-terphenyl (1-2-33).

後処理

  1. dry with materialAfter the organic layer had been dried over anhydrous magnesium sulfate
  2. distillationthe organic solvent was distilled off under reduced pressure
  3. customThe residue was purified by silica gel chromatography (eluent: toluene)
  4. customby recrystallization from a mixed solvent of ethanol and ethyl acetate

出典と根拠

ORDレコード
ord-26b8c37b5a0c4d6a9718589da929de37
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08394468B2

反応ノート

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