Sodium Hydroxide → 4,5-Dihydro-4,10-dioxoimidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylic acid

HRID 1609ノート

反応式

HRID 1609 の反応式
[OH-:1].[Na+].[O:3]=[C:4]1[NH:9][C:8]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=3[CH2:16][C:7]=2[N:6]2[CH:17]=[C:18]([C:20]([O:22]CC)=[O:21])[N:19]=[C:5]12>O1CCOCC1>[O:3]=[C:4]1[NH:9][C:8]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:15]=3[C:16](=[O:1])[C:7]=2[N:6]2[CH:17]=[C:18]([C:20]([OH:22])=[O:21])[N:19]=[C:5]12

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 19691063ethyl 4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate

生成物 1

HCID 196910474,5-Dihydro-4,10-dioxoimidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

5 ml of 1N sodium hydroxide are added to a suspension of 0.2 g of ethyl 4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate in 15 ml of dioxane, and the reaction mixture is stirred vigorously while compressed air is bubbled for 15 hours. After addition of 10 ml of distilled water the mixture is acidified with concentrated hydrochloric acid. The precipitate form is filtered off, washed with water and dried to produce 0.13 g of 4,5-dihydro-4,10-dioxoimidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylic acid in the form of a brown powder whose melting point is higher than 260° C. (1H spectrum in DMSO, T=300K, δ in ppm (200 MHz): between 7.35 and 7.65 (3H, m, CH arom. ), 7.75 (1H, d, J=7 Hz, CH arom.), 8.38 (1H, s, CH arom.), 12.5 (1H, s, NH)).

後処理

  1. customis bubbled for 15 hours
  2. additionAfter addition of 10 ml of distilled water the mixture
  3. filtrationThe precipitate form is filtered off
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-6c6c6d89b5d34913acc93848722ce98e
出典データセット
uspto-grants-1998_03
特許番号
US05726175

反応ノート

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