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Hydrochloric Acid → 3-(3,4,5-Trimethoxybenzoyl)-2-propynyl 3,4,5-trimethoxybenzoate

HRID 1651839
ノート
印刷プレビュー

反応式

HRID 1651839 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6](Cl)=[O:7].[OH:16][CH2:17][C:18]#[C:19][C:20]([C:22]1[CH:27]=[C:26]([O:28][CH3:29])[C:25]([O:30][CH3:31])=[C:24]([O:32][CH3:33])[CH:23]=1)=[O:21].Cl>C(Cl)Cl.N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][CH3:15])[C:11]=1[O:12][CH3:13])[C:6]([O:16][CH2:17][C:18]#[C:19][C:20](=[O:21])[C:22]1[CH:27]=[C:26]([O:28][CH3:29])[C:25]([O:30][CH3:31])=[C:24]([O:32][CH3:33])[CH:23]=1)=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 78282Benzoyl chloride, 3,4,5-trimethoxy-HCID 23050496HCID 23050496、化合物

生成物 1

HCID 230504563-(3,4,5-Trimethoxybenzoyl)-2-propynyl 3,4,5-trimethoxybenzoate

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒
3 回

実験手順

2.21 g (9.59 mmol) of 3,4,5-trimethoxybenzoyl chloride in 10 ml of methylene chloride and 1 ml of pyridine were o added simultaneously at 0° to a solution of 2.0 g (7.99 mmol) of 4-hydroxy-1-(3,4,5-trimethoxyphenyl)-2-butyn-1-one in 25 ml of methylene chloride. The reaction mixture was stirred at 0° for 30 minutes and at room temperature for 1.5 hours, Whereupon 30 ml of 0.5M hydrochloric acid and 100 ml of methylene chloride were added and the aqueous phase was extracted twice with methylene chloride. The combined organic phases were dried over magnesium sulphate and evaporated, and the residue was chromatographed on silica gel with ether. After recrystallization from ethyl acetate/hexane there was obtained 3-(3,4,5-trimethoxybenzoyl)-2-propynyl 3,4,5-trimethoxybenzoate of melting point 106°-108°.

後処理

  1. additionwere added
  2. extractionthe aqueous phase was extracted twice with methylene chloride
  3. dry with materialThe combined organic phases were dried over magnesium sulphate
  4. customevaporated
  5. customthe residue was chromatographed on silica gel with ether
  6. customAfter recrystallization from ethyl acetate/hexane there

出典と根拠

ORDレコード
ord-dfa44755c3b2467ab3068eaf15f72c96
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04929741

反応ノート

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