Methanol → 5-[5-(N-acetyl-anilino)-2, 3-pentadienylidene]-2,7-diphenyl-4-methylpyrazolo[3,4-b]pyridine-3,6-dione

HRID 1073047

반응식

HRID 1073047 반응식
CO.[C:3]1([N:9]2[C:17](=[O:18])[C:16]3[C:15]([CH3:19])=[CH:14][C:13](=[O:20])[N:12]([C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[C:11]=3[NH:10]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.C1(N=[CH:35][CH:36]=[CH:37][CH:38]=[CH:39][NH:40][C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)C=CC=CC=1.[C:47](OC(=O)C)(=[O:49])[CH3:48]>C(N(CC)CC)C>[C:47]([N:40]([CH2:39][CH:38]=[C:37]=[CH:36][CH:35]=[C:14]1[C:13](=[O:20])[N:12]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:11]2=[N:10][N:9]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=3)[C:17](=[O:18])[C:16]2=[C:15]1[CH3:19])[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1)(=[O:49])[CH3:48]

참가 물질

6

반응물 4

HCID 887MethanolHCID 7918Acetic AnhydrideHCID 73902N-(5-(phenylamino)penta-2,5-dienylidene)aniline monohydrochlorideHCID 3603164-methyl-2,7-diphenyl-1H-pyrazolo[3,4-b]pyridine-3,6-dione

생성물 1

HCID 571236985-[5-(N-acetyl-anilino)-2, 3-pentadienylidene]-2,7-diphenyl-4-methylpyrazolo[3,4-b]pyridine-3,6-dione

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

In a solution prepared by adding methanol (50 ml) and triethylamine (2.8 ml) to 2,7-diphenyl-4-methylpyrazolo(3,4-b) pyridine-3,6-dione (3.17 g), 1,7-diphenyl-1,7-diaza-1,3,5-heptatriene hydrochloride (2.85 g) was dissolved and then acetic anhydride (1.88 ml) was added, and the mixture was stirred at room temperature for one hour. The resulting precipitate was collected by filtration, washed with methanol and dried to obtain 5-[5-(N-acetylanilino)-2,3-pentadienylidene]-2,7-diphenyl-4-methylpyrazolo(3,4-b)pyridin-3, 6-dione (1.9). To these crystals (1.5 g), N,N-dimethylformamide (60 ml), 2,7-diphenyl-4-methylpyrazolo(3,4-b)pyridin-3,6-dione (0.95 g) and triethylamine (0.42 g) were added, and stirred at 50° C. for 2 hours. After a trace amount of insoluble matters were removed by filtration, ethyl acetate of 10-fold the volume of the filtrate was added thereto while stirring for crystallization. The resulting crystals were redissolved in a small amount of N,N-dimethylformamide, and a 10-fold volume of ethyl acetate was added thereto for crystallization. The resulting crystals were collected by filtration and dried to obtain compound II-2 (1.3 g). Gold crystals, melting point 300° C. or more, λmaxDMF 792 nm

후처리

  1. customIn a solution prepared
  2. dissolutionwas dissolved
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with methanol
  5. customdried

출처 및 근거

ORD 기록
ord-5d4fb42d68014090b545eac1426edc4c
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968593

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