Diisopropylethylamine → HCID 178487755, 화합물

HRID 1852242노트

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HRID 1852242 반응식
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

참가 물질

6

반응물 3

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

생성물 1

HCID 178487755HCID 178487755, 화합물수율 42.4%

시약·촉매·용매 2

HCID 174Ethylene Glycol용매HCID 962Water용매

반응 조건

온도
145 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-d3cb6ff0c36f4edaaed582a9dc35416b
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957203B2

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