Ethyl isocyanatoacetate → 8-(3-ethoxycarbonylmethylureido)-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one

HRID 481452노트

반응식

HRID 481452 반응식
[NH2:1][C:2]1[CH:18]=[CH:17][C:16]2[C:7]3[NH:8][C:9](=[O:15])[C:10]4[N:11]([CH:12]=[CH:13][N:14]=4)[C:6]=3[CH2:5][C:4]=2[CH:3]=1.[N:19]([CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])=[C:20]=[O:21]>CN(C)C=O>[CH2:26]([O:25][C:23]([CH2:22][NH:19][C:20](=[O:21])[NH:1][C:2]1[CH:18]=[CH:17][C:16]2[C:7]3[NH:8][C:9](=[O:15])[C:10]4[N:11]([CH:12]=[CH:13][N:14]=4)[C:6]=3[CH2:5][C:4]=2[CH:3]=1)=[O:24])[CH3:27]

참가 물질

4

반응물 2

HCID 76283Ethyl isocyanatoacetateHCID 189753948-amino-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one

생성물 1

HCID 190660338-(3-ethoxycarbonylmethylureido)-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

The preparation is carried out as in Example 7, from 3 g of 8-amino-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one and 2 times 2.8 ml of ethyl 2-isocyanatoacetate in 170 ml of dimethylformamide. The insoluble material thus obtained is filtered and recrystallized from dimethylformamide. After filtration, washing with water and drying under reduced pressure (1 mm Hg, 0.13 kPa) at 60° C., there are obtained 2.6 g of 8-(3-ethoxycarbonylmethylureido)-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-4-one in the form of a pink solid, the melting point of which is greater than 260° C. (Analysis C18H17N5 O4.0.75H2O.0.20DMF, % calculated C: 58.85, H: 4.66, N: 19.06, % found C: 58.9, H: 5.0, N: 18.9).

후처리

  1. customThe insoluble material thus obtained
  2. filtrationis filtered
  3. customrecrystallized from dimethylformamide
  4. filtrationAfter filtration
  5. washwashing with water
  6. customdrying under reduced pressure (1 mm Hg, 0.13 kPa) at 60° C.

출처 및 근거

ORD 기록
ord-62ba3847281f4d51bde9784d112e1af8
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05789406

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