Hydrazine hydrate (1:1) → (2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-amine

HRID 70706노트

반응식

HRID 70706 반응식
O.NN.[C:4]([C:8]1[CH:13]=[CH:12][C:11](/[C:14](/[C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[C:30]([O:35][CH3:36])[N:29]=2)=[CH:15]\[CH2:16][N:17]2C(=O)C3C(=CC=CC=3)C2=O)=[CH:10][CH:9]=1)([CH3:7])([CH3:6])[CH3:5]>C(O)C.[Cl-].[Na+].O>[C:4]([C:8]1[CH:13]=[CH:12][C:11](/[C:14](/[C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[C:30]([O:35][CH3:36])[N:29]=2)=[CH:15]\[CH2:16][NH2:17])=[CH:10][CH:9]=1)([CH3:7])([CH3:5])[CH3:6]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 67398370HCID 67398370, 화합물

생성물 1

HCID 67400678(2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-amine

시약·촉매·용매 2

HCID 702Ethanol용매HCID 57417360Sodium chloride; water용매

실험 절차

Hydrazine monohydrate (13 μL) was added to a solution of 2-[(2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-yl]-1H-isoindole-1,3(2H)-dione (98 mg) in ethanol. Thereafter, the mixture was stirred with heating under reflux for three hours and then stirred at room temperature overnight. Brine was added to the reaction solution, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure to give a crude product of (2E)-3-(4-tert-butylphenyl)-3-(5-chloro-6-methoxypyridin-2-yl)prop-2-en-1-amine.

후처리

  1. temperaturewith heating
  2. temperatureunder reflux for three hours
  3. stirringstirred at room temperature overnight
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customafter which the solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3d581e25f87646a4b58c552ec8c5e56a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822503B2

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