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Isobutylamine → 4-Amino-N-[2-(isobutylamino)ethyl]-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-7,8-dihydro-2H-6-thia-1,2,3,5-tetraazaacenaphthylene-7-carboxamide

HRID 1693278
ノート
印刷プレビュー

反応式

HRID 1693278 の反応式
[NH2:1][C:2]1[N:3]=[C:4]2[C:13]3[C:7]([CH2:8][CH:9]([C:14]([NH:16][CH2:17][CH2:18]Cl)=[O:15])[S:10][C:11]=3[N:12]=1)=[N:6][N:5]2[CH2:20][C:21]1[C:26]([CH3:27])=[C:25]([O:28][CH3:29])[C:24]([CH3:30])=[CH:23][N:22]=1.[CH2:31]([NH2:35])[CH:32]([CH3:34])[CH3:33]>O1CCOCC1>[NH2:1][C:2]1[N:3]=[C:4]2[C:13]3[C:7]([CH2:8][CH:9]([C:14]([NH:16][CH2:17][CH2:18][NH:35][CH2:31][CH:32]([CH3:34])[CH3:33])=[O:15])[S:10][C:11]=3[N:12]=1)=[N:6][N:5]2[CH2:20][C:21]1[C:26]([CH3:27])=[C:25]([O:28][CH3:29])[C:24]([CH3:30])=[CH:23][N:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6558IsobutylamineHCID 593114214-Amino-N-(2-chloroethyl)-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-7,8-dihydro-2H-6-thia-1,2,3,5-tetraazaacenaphthylene-7-carboxamide

生成物 1

HCID 593115264-Amino-N-[2-(isobutylamino)ethyl]-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-7,8-dihydro-2H-6-thia-1,2,3,5-tetraazaacenaphthylene-7-carboxamide収率 28%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture composed of 4-amino-N-(2-chloroethyl)-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-7,8-dihydro-2H-6-thia-1,2,3,5-tetraazaacenaphthylene-7-carboxamide of Example 16 (20 mg), isobutylamine (0.8 mL) and dioxane (3 mL) was heated under reflux for 16 hours, and then the reaction mixture was concentrated under reduced pressure. The resulting residue was purified by reversed phase liquid chromatography to obtain the title compound (6 mg, 28%) as a solid.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. customThe resulting residue was purified by reversed phase liquid chromatography

出典と根拠

ORDレコード
ord-5047bebc846a4beeb484a079586b4651
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158638B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート