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Hydrogen Bromide → HCID 58452756、化合物

HRID 70648
ノート
印刷プレビュー

反応式

HRID 70648 の反応式
Br.[NH2:2][C:3]1[CH:4]=[CH:5][C:6](/[C:11](/[C:19]2[CH:24]=[CH:23][C:22]([C:25]([CH3:28])([CH3:27])[CH3:26])=[CH:21][CH:20]=2)=[CH:12]/[C@@H:13]2[NH:17][C:16](=[O:18])[CH2:15][CH2:14]2)=[N:7][C:8]=1[O:9]C.O>O1CCOCC1>[NH2:2][C:3]1[C:8](=[O:9])[NH:7][C:6](/[C:11](/[C:19]2[CH:20]=[CH:21][C:22]([C:25]([CH3:27])([CH3:26])[CH3:28])=[CH:23][CH:24]=2)=[CH:12]/[C@H:13]2[CH2:14][CH2:15][C:16](=[O:18])[NH:17]2)=[CH:5][CH:4]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 260Hydrogen BromideHCID 962WaterHCID 67399550HCID 67399550、化合物

生成物 1

HCID 58452756HCID 58452756、化合物収率 44%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
65 °C

実験手順

48% hydrobromic acid (0.5 mL) was added to a solution of (5R)-5-[(E)-2-(5-amino-6-methoxypyridin-2-yl)-2-(4-tert-butylphenyl)ethenyl]pyrrolidin-2-one (20 mg) in 1,4-dioxane (1 mL), and the mixture was stirred at 65° C. for 30 minutes. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=10:0→4:1) and crystallized from chloroform-ethyl acetate to give the title compound as a light brown powder (8 mg, 44%).

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. customafter which the solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (chloroform:methanol=10:0→4:1)
  6. customcrystallized from chloroform-ethyl acetate

出典と根拠

ORDレコード
ord-87d8b283ec21442a9b8bd1ccb7a69448
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822503B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート