Hydrochloric Acid → HCID 67398266、化合物

HRID 70707ノート

反応式

HRID 70707 の反応式
[C:1](OC(=O)C)(=[O:3])[CH3:2].[C:8]([C:12]1[CH:17]=[CH:16][C:15](/[C:18](/[C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([O:29][CH3:30])[N:23]=2)=[CH:19]\[CH2:20][NH2:21])=[CH:14][CH:13]=1)([CH3:11])([CH3:10])[CH3:9].Cl>N1C=CC=CC=1>[C:8]([C:12]1[CH:17]=[CH:16][C:15](/[C:18](/[C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([O:29][CH3:30])[N:23]=2)=[CH:19]\[CH2:20][NH:21][C:1](=[O:3])[CH3:2])=[CH:14][CH:13]=1)([CH3:11])([CH3:9])[CH3:10]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 67400678(2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-amine

生成物 1

HCID 67398266HCID 67398266、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Acetic anhydride (21 μL) was added to a solution of (2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-amine in pyridine (1 mL), and the mixture was stirred at room temperature for 1.5 hours. 1 M hydrochloric acid was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1→1:1) to give N-[(2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-yl]acetamide as a pale yellow amorphous (50 mg, 67% (two steps)).

後処理

  1. extractionfollowed by extraction with chloroform
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. customafter which the solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1→1:1)

出典と根拠

ORDレコード
ord-e94b963794564c15b4f412c4a15d65fd
出典データセット
uspto-grants-2014_09
特許番号
US08822503B2

反応ノート

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