Diisopropylethylamine → HCID 178487755、化合物

HRID 1852242ノート

反応式

HRID 1852242 の反応式
Br[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH3:13])[CH:10]=2)[C:5](=[O:14])[NH:4][CH:3]=1.[N:15]1([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1.CCN(C(C)C)C(C)C>C(O)CO.O>[OH:14][C:5]1[C:6]2[C:11](=[CH:10][C:9]([O:12][CH3:13])=[CH:8][CH:7]=2)[C:2]([N:18]2[CH2:17][CH2:16][N:15]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:20][CH2:19]2)=[CH:3][N:4]=1

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 579564624-Bromo-6-methoxyisoquinolin-1(2H)-one

生成物 1

HCID 178487755HCID 178487755、化合物収率 42.4%

試薬・触媒・溶媒 2

HCID 174Ethylene Glycol溶媒HCID 962Water溶媒

反応条件

温度
145 °C

実験手順

To a solution of 4-bromo-6-methoxyisoquinolin-1(2H)-one (0.5 g, 1.968 mmol) and tert-butyl piperazine-1-carboxylate (0.916 g, 4.92 mmol) in ethylene glycol (5 ml) was added DIPEA (1.0.31 ml, 5.90 mmol) and heated to 145° C. for overnight in sealed tube. The reaction mixture was diluted with water and extracted with ethyl acetate. Combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to get crude compound (0.3 g, 29.4%). The crude compound was taken for the next step without further purification. MS: MS m/z 260.20 (M++1).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialCombined organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-d3cb6ff0c36f4edaaed582a9dc35416b
出典データセット
uspto-grants-2015_02
特許番号
US08957203B2

反応ノート

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