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Hydrochloric Acid → HCID 67285452, 화합물

HRID 1943535
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HRID 1943535 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

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

생성물 1

HCID 67285452HCID 67285452, 화합물

시약·촉매·용매 2

HCID 314042,6-Di-tert-butyl-4-methylphenol촉매HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-26b8c37b5a0c4d6a9718589da929de37
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394468B2

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