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

HRID 1609노트

반응식

HRID 1609 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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)).

후처리

  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

출처 및 근거

ORD 기록
ord-6c6c6d89b5d34913acc93848722ce98e
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726175

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