K-252C → Ngic-I

HRID 2395706

반응식

HRID 2395706 반응식
[O:1]=[C:2]1[C:6]2[C:7]3[C:24]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[NH:18][C:8]=3[C:9]3[NH:10][C:11]4[C:16]([C:17]=3[C:5]=2[CH2:4][NH:3]1)=[CH:15][CH:14]=[CH:13][CH:12]=4.[CH3:25][CH2:26][CH2:27]CCCC=CCCC.C(#[N:38])C>>[C:27]([CH2:26][CH2:25][N:10]1[C:9]2[C:8]3[NH:18][C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][C:24]=4[C:7]=3[C:6]3[C:2](=[O:1])[NH:3][CH2:4][C:5]=3[C:17]=2[C:16]2[C:11]1=[CH:12][CH:13]=[CH:14][CH:15]=2)#[N:38]

참가 물질

4

반응물 3

HCID 3815K-252CHCID 6342AcetonitrileHCID 136496Undec-4-ene

생성물 1

HCID 3714Ngic-I

반응 조건

온도
20 °C

실험 절차

300 mg (0.96 mmole) 6,7,12,13-tetrahydro-5-oxo-5H-indolo[2.3-a]pyrrolo [3,4-c]carbazole, suspended in 20 mL acetonitrile, are mixed with 0.3 mL (4.56 mole) acrylic acid nitrile and 2 drops of 1,8-diazabicyclo[5,4,0[undec-7-ene (DBU) and stirred for 3 days at 20° C. The mixture of starting materials and product is filtered off, again mixed with the same amounts of acrylic acid nitrile, DBU and acetonitrile and stirred for a further 3 days at 20° C. After again repeating this procedure and after a further 3 days at 20° C., the 12-(2-cyanoethyl)-6,7,12, 13-tetrahydro-5-oxo-5H-indolo[2,3-a]pyrrolo[3,4-c]carbazole is filtered off in the form of beige colored crystals which decompose above 275° C.

후처리

  1. additionThe mixture of starting materials and product
  2. filtrationis filtered off
  3. additionagain mixed with the same amounts of acrylic acid nitrile, DBU and acetonitrile
  4. stirringstirred for a further 3 days at 20° C
  5. waitafter a further 3 days at 20° C.
  6. filtrationthe 12-(2-cyanoethyl)-6,7,12, 13-tetrahydro-5-oxo-5H-indolo[2,3-a]pyrrolo[3,4-c]carbazole is filtered off in the form of beige colored crystals which
  7. customdecompose above 275° C.

출처 및 근거

ORD 기록
ord-88f9310c8bde4528a8005ced7eac3c75
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05489608

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