n-[2-(Ethylamino)ethyl]phthalimide hydrochloride salt → N-[2-(ethylamino)ethyl]phthalimide

HRID 2273613ノート

反応式

HRID 2273613 の反応式
Cl.[CH2:2]([NH:4][CH2:5][CH2:6][N:7]1[C:11](=[O:12])[C:10]2=[CH:13][CH:14]=[CH:15][CH:16]=[C:9]2[C:8]1=[O:17])[CH3:3]>ClCCl>[CH2:2]([NH:4][CH2:5][CH2:6][N:7]1[C:11](=[O:12])[C:10]2=[CH:13][CH:14]=[CH:15][CH:16]=[C:9]2[C:8]1=[O:17])[CH3:3]

参加物

3

反応物 1

HCID 66944064n-[2-(Ethylamino)ethyl]phthalimide hydrochloride salt

生成物 1

HCID 21748445N-[2-(ethylamino)ethyl]phthalimide収率 82.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A suspension of N-[2-(ethylamino)ethyl]phthalimide hydrochloride salt (1) (2.00 g, 7.86 mmol) (Jones, J. H.; Holtz, W. J.; Cragoe, E. J. 6-Substituted 5-chloro-1,3-dihydro-2H-imidazo[4,5-b]pyrazin-2-ones with hypotensive activity. J. Med. Chem. 1973, 16, 537-42) in dichloromethane (100 mL) was washed with a 5% aqueous sodium carbonate solution (5 mL). The mixture was extracted with dichloromethane (40 mL). The organic layers were combined, dried on magnesium sulfate, filtered and evaporated under vacuum to give compound 2 (1.41 g, 6.47 mmol) as a yellow solid. Yield 82%; mp 111-113° C. (dec.); IR (KBr) ν 1292, 1395, 1430, 1541, 1637, 1712, 2929, 3200-3600 cm−; 1H NMR (200 MHz, CDCl3) δ 1.07 (t, 3H, J=7.1 Hz), 2.68 (q, 2H, J=7.1 Hz), 2.92 (t, 2H, J=6.5 Hz), 3.81 (t, 2H, J=6.5 Hz), 7.68 (m, 2H), 7.82 (m, 2H).

後処理

  1. washwas washed with a 5% aqueous sodium carbonate solution (5 mL)
  2. extractionThe mixture was extracted with dichloromethane (40 mL)
  3. customdried on magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under vacuum

出典と根拠

ORDレコード
ord-ba18e9ec766f40c8a836881a6ff5a542
出典データセット
uspto-grants-2015_09
特許番号
US09125937B2

反応ノート

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