Hydrochloric Acid → HCID 67398266, 화합물

HRID 70707노트

반응식

HRID 70707 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 67398266HCID 67398266, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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)).

후처리

  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)

출처 및 근거

ORD 기록
ord-e94b963794564c15b4f412c4a15d65fd
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822503B2

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