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Pyridine → HCID 23050454, 화합물

HRID 1651838
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HRID 1651838 반응식
[C:1](Cl)(=[O:3])[CH3:2].N1C=CC=CC=1.[OH:11][CH2:12][C:13]#[C:14][C:15]([C:17]1[CH:22]=[C:21]([O:23][CH3:24])[C:20]([O:25][CH3:26])=[C:19]([O:27][CH3:28])[CH:18]=1)=[O:16].P([O-])([O-])([O-])=O>C(Cl)Cl>[C:1]([O:11][CH2:12][C:13]#[C:14][C:15](=[O:16])[C:17]1[CH:18]=[C:19]([O:27][CH3:28])[C:20]([O:25][CH3:26])=[C:21]([O:23][CH3:24])[CH:22]=1)(=[O:3])[CH3:2]
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참가 물질

6

반응물 4

HCID 1049PyridineHCID 1061PhosphateHCID 6367Acetyl chlorideHCID 23050496HCID 23050496, 화합물

생성물 1

HCID 23050454HCID 23050454, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.815 g of acetyl chloride and 0.827 g of pyridine were added simultaneously to a solution of 2.0 g (7.99 mmol) of 4-hydroxy-1-(3,4,5-trimethoxyphenyl)-2-butyn-1-one in 20 ml of methylene chloride. The reaction mixture was stirred at 0° for 1 hour, whereupon it was treated with 30 ml of phosphate buffer (pH 6) and the aqueous phase was extracted twice with methylene chloride. The combined organic phases were dried over magnesium sulphate and evaporated. The residue was recrystallized from ethyl acetate/hexane and there was obtained 3-(3,4,5-trimethoxy-benzoyl)-2-propynyl acetate of melting point 104°-105°.

후처리

  1. extractionthe aqueous phase was extracted twice with methylene chloride
  2. dry with materialThe combined organic phases were dried over magnesium sulphate
  3. customevaporated
  4. customThe residue was recrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-7be08d16adc846fd87120a5d5bed18b8
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04929741

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