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

HRID 70706ノート

反応式

HRID 70706 の反応式
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]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 67398370HCID 67398370、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d581e25f87646a4b58c552ec8c5e56a
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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