Acetic Acid → 12-(2-Cyanoethyl)-6,7,12,13-tetrahydro-7-methoxy-13-methyl-5-oxo-5H-indolo[2,3-a]pyrrolo[3,4-c]carbazole

HRID 2395710

반응식

HRID 2395710 반응식
[C:1]([CH2:3][CH2:4][N:5]1[C:17]2[C:16]3[N:18]([CH3:25])[C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][C:24]=4[C:15]=3[C:14]3[C:26](=[O:29])[NH:27][CH2:28][C:13]=3[C:12]=2[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)#[N:2].[C:30](O)(=[O:32])C>CO>[C:1]([CH2:3][CH2:4][N:5]1[C:17]2[C:16]3[N:18]([CH3:25])[C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][C:24]=4[C:15]=3[C:14]3[C:26](=[O:29])[NH:27][CH:28]([O:32][CH3:30])[C:13]=3[C:12]=2[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)#[N:2]

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 350112-(2-cyanoethyl)-6,7,12,13-tetrahydro-13-methyl-5-oxo-5H-indolo(2,3-a)pyrrolo(3,4-c)carbazole

생성물 1

HCID 1898988812-(2-Cyanoethyl)-6,7,12,13-tetrahydro-7-methoxy-13-methyl-5-oxo-5H-indolo[2,3-a]pyrrolo[3,4-c]carbazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

356 mg (0.94 mmole) 12-(2-cyanoethyl)-6,7,12,13-tetrahydro-13-methyl-5-oxo-5H-indolo[2,3a]pyrrolo[3,4-c]carbazole (Example 2) are stirred for 16 hours at 20° C. in 50 mL glacial acetic acid and 1 mL methanol. The further preparation is carried out in Example 4 and the crude product is chromatographed on silica gel with dichloromethane/methanol 199:1 (v/v). The fraction with an Rf of 0.25 in toluene/ethyl acetate 4:1 (v/v) is isolated. 12-(2-Cyanoethyl)-6,7,12,13-tetrahydro-7-methoxy-13-methyl-5-oxo-5H-indolo[2,3-a]pyrrolo[3,4-c]carbazole is obtained in the form of beige crystals which decompose above about 200° C.

후처리

  1. customThe further preparation
  2. customthe crude product is chromatographed on silica gel with dichloromethane/methanol 199:1 (v/v)
  3. customThe fraction with an Rf of 0.25 in toluene/ethyl acetate 4:1 (v/v) is isolated

출처 및 근거

ORD 기록
ord-e0b5c16f9e0749198ea8ec85f5807443
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05489608

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