Sodium Hydroxide → HCID 67399735、化合物

HRID 70603ノート

反応式

HRID 70603 の反応式
O.NN.[CH:4]1([C:7]2[CH:8]=[CH:9][C:10](/[C:15](/[C:30]3[CH:35]=[CH:34][C:33]([S:36][CH3:37])=[CH:32][CH:31]=3)=[CH:16]/[CH2:17][CH2:18][N:19]3C(=O)C4C(=CC=CC=4)C3=O)=[N:11][C:12]=2[O:13][CH3:14])[CH2:6][CH2:5]1.[OH-].[Na+]>C(O)C>[CH:4]1([C:7]2[CH:8]=[CH:9][C:10](/[C:15](/[C:30]3[CH:35]=[CH:34][C:33]([S:36][CH3:37])=[CH:32][CH:31]=3)=[CH:16]/[CH2:17][CH2:18][NH2:19])=[N:11][C:12]=2[O:13][CH3:14])[CH2:6][CH2:5]1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 674002742-{(3E)-4-(5-cyclopropyl-6-methoxypyridin-2-yl)-4-[4-(methylsulfanyl)phenyl]but-3-en-1-yl}-1H-isoindole-1,3(2H)-dione

生成物 1

HCID 67399735HCID 67399735、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
95 °C

実験手順

Hydrazine monohydrate (1 mL) was added to a solution of 2-{(3E)-4-(5-cyclopropyl-6-methoxypyridin-2-yl)-4-[4-(methylsulfanyl)phenyl]but-3-en-1-yl}-1H-isoindole-1,3(2H)-dione (320 mg) in ethanol (4 mL), and the mixture was stirred at 95° C. for one hour. The reaction solution was poured into a 3 M sodium hydroxide solution, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure to give (3E)-4-(5-cyclopropyl-6-methoxypyridin-2-yl)-4-[4-(methylsulfanyl)phenyl]but-3-en-1-amine as a colorless amorphous (225 mg, 97%).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customafter which the solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-dbf7988bd3ec4d628f3d942f5381f4fb
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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